Publications by authors named "Hiroki Nagashima"

40 Publications

"Salvage techniques" are the key to overcome difficult biliary cannulation in endoscopic retrograde cholangiopancreatography.

Sci Rep 2022 Aug 10;12(1):13627. Epub 2022 Aug 10.

Department of Gastroenterology, Graduate School of Medicine, Chiba University, Inohana 1-8-1, Chiba-City, 260-8670, Japan.

Although the efficacy and safety of salvage techniques for biliary cannulation in endoscopic retrograde cholangiopancreatography (ERCP) have been reported, few reports analyzed the choice of techniques and their clinical outcomes in large cohorts. This study aimed to evaluate the outcomes of biliary cannulation in patients with native papillae. We retrospectively identified 1021 patients who underwent initial ERCP from January 2013 to March 2020. We investigated background factors, treatment details, cannulation success rates, and adverse event rates. Then we analyzed a series of treatment processes, including salvage techniques such as double guidewire technique (DGT), needle knife pre-cutting (NKP), and transpancreatic pre-cut papillotomy (TPPP). The initial ERCP success rate using standard technique alone was 62.8%, which increased to 94.3% including salvage techniques. Salvage techniques were frequently required in patients with long oral protrusions (OR 2.38; 95% CI 1.80-3.15; p < 0.001). A total of 503 cases (49.3%) had long oral protrusions, 47.5% of which required the salvage techniques, much higher than 27.5% of not-long cases. Patients with long oral protrusions had a higher frequency of NKP. In conclusion, patients with long oral protrusions frequently required salvage techniques. Salvage techniques may help to overcome many difficult biliary cannulation cases.
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http://dx.doi.org/10.1038/s41598-022-17809-5DOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC9365799PMC
August 2022

Successful endoscopic retrieval of a migrated pancreatic stent using a basket catheter for peroral cholangioscopy through a biliary plastic stent pusher tube: a case report.

J Rural Med 2022 Jul 1;17(3):189-192. Epub 2022 Jul 1.

Department of Gastroenterology, Graduate School of Medicine, Chiba University, Japan.

Retrieval is challenging once prophylactic pancreatic stents migrate deep into the pancreatic duct. Herein, we describe a case of successful endoscopic retrieval of a migrated prophylactic pancreatic stent using a basket catheter through a biliary plastic stent pusher tube. A 71 year-old man was referred to our hospital for removal of a straight-shaped migrated 5-Fr 3-cm prophylactic pancreatic stent with a flap on the duodenal side. There were no subjective symptoms at the time of the hospital visit. During endoscopic retrograde cholangiopancreatography, we inserted an 8.5-Fr plastic biliary stent pusher tube in front of the migrated pancreatic stent. The stent was then grasped using a basket catheter for peroral cholangioscopy through the biliary stent pusher tube. The stent was pulled into the pusher tube and was successfully retrieved from the pancreatic duct. No complications were associated with endoscopic retrograde cholangiopancreatography. Although rare, prophylactic pancreatic duct stent migration after pancreatic duct guidewire placement should be noted. In our case, endoscopic retrieval of a migrated prophylactic pancreatic stent using a basket catheter for peroral cholangioscopy through the biliary plastic stent pusher tube was successful.
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http://dx.doi.org/10.2185/jrm.2022-003DOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC9263960PMC
July 2022

Intraperitoneal bleeding from the right gastroepiploic artery by endoscopic ultrasonography: a case report.

J Rural Med 2022 Jul 1;17(3):184-188. Epub 2022 Jul 1.

Department of Gastroenterology, Graduate School of Medicine, Chiba University, Japan.

To describe the case of a patient with intraperitoneal bleeding from the gastroepiploic artery by endoscopic ultrasound who was successfully treated with transcatheter arterial coil embolization. An 87-year-old man was referred to our hospital for examination of a gallbladder tumor. Endoscopic ultrasonography was performed using an oblique-view echoendoscope. After the endoscopic ultrasound, the patient went into shock. Computed tomography revealed a huge intraperitoneal hematoma and an aneurysm in the right gastroepiploic artery that were not seen on previous computed tomography images. Thus, urgent catheter angiography was performed, which showed a pseudoaneurysm of the right gastroepiploic artery and extravasation of the contrast medium from the pseudoaneurysm. Transcatheter arterial coil embolization was subsequently performed, and the bleeding stopped. Thereafter, his hemodynamics stabilized and his general condition improved. The patient was discharged 22 days post-treatment with an uneventful course. Observation-only endoscopic ultrasound without invasive procedures can cause intraperitoneal bleeding due to a ruptured splanchnic artery. Thus, endoscopic ultrasonography should be performed more carefully in elderly patients.
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http://dx.doi.org/10.2185/jrm.2022-002DOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC9263947PMC
July 2022

Chemical reactions of graphitic carbon nitride films with glass surfaces and their impact on photocatalytic activity.

Phys Chem Chem Phys 2022 Jul 27;24(29):17504-17515. Epub 2022 Jul 27.

National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology, Central 5, 1-1-1 Higashi, Tsukuba, Ibaraki 305-8565, Japan.

Thin films of graphitic carbon nitride (g-CN), a visible-light-driven photocatalyst, have recently attracted interest for application in photoelectrochemical cells for water splitting and high-throughput photocatalysis. In typical syntheses, g-CN films are formed by heating the nitrogen-rich precursor and substrate to 500-600 °C. The heated substrate should affect the polycondensation of the precursor and thereby alter the properties of the g-CN film. In this paper, we demonstrate that soda-lime glass, such as commercial glass slides, modifies the chemical structure of g-CN. The terminal amino groups of g-CN are partially substituted with cyanamide and hydroxyl groups. The electron-withdrawing groups provide the energy offsets of the frontier orbitals between the modified and unmodified molecules, facilitating exciton dissociation. After alkali metals are removed, the modified g-CN film exhibits a faster photodegradation of methyl orange compared with a melon film. The simple protocol to activate a g-CN film without co-catalysts paves a new way to enhance photocatalytic activity selections of substrates, including waste glass.
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http://dx.doi.org/10.1039/d2cp01677jDOI Listing
July 2022

Successful endoscopic treatment of huge infected biloma and hepatic abscess after endoscopic ultrasound-guided hepaticogastrostomy with brain abscess.

Clin J Gastroenterol 2022 Jun 28. Epub 2022 Jun 28.

Department of Gastroenterology, Graduate School of Medicine, Chiba University, 1-8-1 Inohana, Chuo-ku, Chiba, 260-8670, Japan.

A 77-year-old woman with obstructive jaundice due to pancreatic head tumor was admitted to our hospital for biliary drainage. Transpapillary biliary drainage was attempted using endoscopic retrograde cholangiopancreatography; however, the catheter could not be inserted into the bile duct. Endoscopic ultrasound-guided hepaticogastrostomy (EUS-HGS) was conducted using a 7-Fr plastic stent. Fever and cognitive dysfunction were observed 73 days after EUS-HGS. Abdominal-computed tomography (CT) showed a huge biloma and a liver abscess. On admission, an uncovered metal stent was applied to the biliary obstruction site of the distal bile duct using an antegrade stenting technique, and the plastic hepaticogastrostomy stent was substituted with a new one. On the second day, two double-pigtail plastic stents were inserted into the biloma, and one into the liver abscess. Head CT and magnetic resonance imaging revealed a brain abscess in the right cerebral frontal lobe. Serum white blood cell count and C-reactive protein level, and the state of consciousness, improved with antibiotic administration. Biloma and liver abscess almost disappeared on CT 38 days after admission. The brain abscess also improved, and the patient was discharged from the hospital 48 days after admission. Endoscopic ultrasound-guided biloma drainage is helpful because self-removal of the drainage tube and reduced activities of daily living are unlikely to occur.
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http://dx.doi.org/10.1007/s12328-022-01659-9DOI Listing
June 2022

Feasibility of a Single Pigtail Stent Made by Cutting a Nasobiliary Drainage Tube in Endoscopic Transpapillary Gallbladder Stenting for Acute Cholecystitis.

Cureus 2022 May 17;14(5):e25072. Epub 2022 May 17.

Gastroenterology, Chiba University, Chiba, JPN.

Background and objective In this study, we aimed to evaluate the efficacy and safety of a single pigtail stent made by cutting a nasobiliary drainage tube (NBD stent) by comparing the clinical outcomes of using an NBD stent and those of using a ready-made double pigtail stent (RDP stent) in endoscopic gallbladder stenting (EGBS) for acute cholecystitis. Materials and methods This was a single-center retrospective study involving 20 cases that had technical success with EGBS for acute cholecystitis; the patients were divided into two groups: those using NBD stent (NBD group) and those using RDP stent (RDP group). The baseline characteristics and clinical outcomes were compared between the two groups. Results There were 13 patients in the NBD group and seven in the RDP group. The rates of clinical success (NBD group: 92% vs. RDP group: 100%, p=0.45) did not differ significantly between the groups. Regarding adverse events, gallbladder perforation occurred in one case in the NBD group; however, no other adverse events occurred in either group (NBD group: 7.7% vs. RDP group: 0%, p=0.45). The stent patency periods did not differ significantly between the groups [NBD group: 43 (12-64) days vs. RDP group: 97 (58-215) days, p=0.17]. The stent patency period in cases of long-term stent placement after EGBS was 1,381 days and 1,579 days in the NBD group and 305 days in the RDP group, respectively. Conclusion NBD stents are considered as effective as RDP stents in EGBS for acute cholecystitis. They are highly versatile and can be used for both bridging to surgery and long-term stent placement.
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http://dx.doi.org/10.7759/cureus.25072DOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC9202489PMC
May 2022

Liver cirrhosis is a risk factor for poor prognosis of acute cholangitis caused by choledocholithiasis.

Ann Hepatol 2022 May-Jun;27(3):100696. Epub 2022 Mar 5.

Department of Gastroenterology, Graduate School of Medicine, Chiba University, 1-8-1 Inohana, Chuo-ku, Chiba-shi, Chiba 260-8677, Japan. Electronic address:

Introduction And Objectives: Acute cholangitis, which is characterized by biliary infection and acute liver injury, may impact cirrhosis prognosis. However, the prognosis itself remains unclear.

Materials And Methods: This multicenter retrospective cohort study compared the mortality and liver function change between patients with and without cirrhosis who underwent endoscopic treatment for acute cholangitis caused by choledocholithiasis between January 2004 and December 2019.

Results: We analyzed 699 patients, 44 of whom had cirrhosis. The cirrhotic group had a significantly higher 30-day mortality rate than the noncirrhotic group (14% vs. 1%; P < 0.001). The cirrhotic group also had significantly lower total bilirubin and albumin recovery. However, all patients with cirrhosis who survived achieved total-bilirubin recovery, and 91% achieved albumin recovery within 90 days. In multivariable Cox regression analysis, the independent risk factors for total-bilirubin recovery included cirrhosis (hazard ratio, 0.37; 95%CI, 0.24‒0.58; P < 0.001) and high total-bilirubin level (0.46; 95%CI, 0.34‒0.60; P < 0.001), whereas those for albumin recovery were cirrhosis (0.51; 95%CI, 0.33‒0.79; P = 0.002), high age (0.62; 95%CI, 0.47‒0.82; P < 0.001), organ dysfunction (0.62; 95%CI, 0.39‒0.96; P = 0.03), low albumin level (0.57; 95%CI, 0.36‒0.91; P = 0.02), and high C-reactive protein level (0.73; 95%CI, 0.56‒0.95; P = 0.02).

Conclusions: Patients with cirrhosis complicated with acute cholangitis had poor prognosis. Recovery of liver function after endoscopic treatment was slow; nevertheless, most patients who survived could recover within 90 days.
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http://dx.doi.org/10.1016/j.aohep.2022.100696DOI Listing
May 2022

Diagnostic value of IMP3 and p53 immunohistochemical staining in EUS-guided fine-needle aspiration for solid pancreatic tumors.

Sci Rep 2021 08 26;11(1):17257. Epub 2021 Aug 26.

Department of Gastroenterology, Chiba University Graduate School of Medicine, 1-8-1 Inohana, Chuo-ku, Chiba, 260-8670, Japan.

We previously identified insulin-like growth factor-II messenger ribonucleic acid-binding protein 3 (IMP3) as a valuable marker to distinguish malignant from benign lesions in pancreatic solid masses. The aim of this prospective study was to evaluate the usefulness of IMP3 and p53 immunohistochemical staining in endoscopic ultrasound-guided fine-needle aspiration (EUS-FNA) samples for pancreatic solid masses. The study recruited 90 consecutive patients with pancreatic masses, including 62 pancreatic ductal adenocarcinomas (PDACs), 11 benign tumors, and 17 other tumors, who underwent EUS-FNA, and conducted IMP3 and p53 immunohistochemical staining. The main outcome measurement was improved diagnostic utility using IMP3 and p53 immunohistochemical staining. IMP3 and p53 expressions were detected in 60.8% and 49.4% of malignant lesions, 69.4% and 58.1% of PDACs, and 0% of benign lesions, respectively. In PDAC and benign tumors, the use of IMP3 and/or p53 immunostaining increased the sensitivity of cytohistological analysis from 88.7 to 93.5%, although the difference was not statistically significant. The sensitivity of histological analysis combined with that of IMP3 staining was 91.9%, which was significantly greater than that of histology alone (80.6%). The use of IMP3 and p53 immunohistochemical staining did not significantly improve the sensitivity of cytohistological analysis; however, IMP3 staining may be helpful for the histological analysis of malignant pancreatic tumors.
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http://dx.doi.org/10.1038/s41598-021-96492-4DOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC8390649PMC
August 2021

Diagnostic value of peroral cholangioscopy in addition to computed tomography for indeterminate biliary strictures.

Surg Endosc 2022 05 9;36(5):3408-3417. Epub 2021 Aug 9.

Department of Gastroenterology, Graduate School of Medicine, Chiba University, Inohana 1-8-1, Chiba-City, Chiba, 260-8670, Japan.

Background: Peroral cholangioscopy (POCS) has been used to overcome the difficulty in diagnosing indeterminate biliary stricture or tumor spread. However, the value of adding POCS to computed tomography (CT) remains unclear. Our aim was to evaluate the diagnostic value of adding POCS to CT for indeterminate biliary stricture and tumor spread by interpretation of images focusing on the high diagnostic accuracy of visual findings in POCS.

Methods: We retrospectively identified 52 patients with biliary stricture who underwent endoscopic retrograde cholangiography (ERC) at our institution between January 2013 and December 2018. Two teams, each composed of an expert endoscopist and surgeon, performed the interpretation independently, referring to the CT findings of the radiologist. The CT + ERC + POCS images (POCS group) were evaluated 4 weeks after the evaluation of CT + ERC images (CT group). A 5-point scale (1: definitely benign to 5: definitely malignant) was used to determine the confident diagnosis rate, which was defined as an evaluation value of 1 or 5. Tumor spread was also evaluated.

Results: In the evaluation of 45 malignant diagnoses, the score was significantly closer to 5 in the POCS group than in the CT group in both teams (P < 0.001). The confident diagnosis rate was significantly higher for the POCS group (92% and 73%) than for the CT group (25% and 12%) in teams 1 and 2, respectively (P < 0.001). We found no significant difference in diagnostic accuracy for tumor spread between the groups.

Conclusion: Visual POCS findings confirmed the diagnosis of biliary strictures. POCS was useful in cases of indefinite diagnosis of biliary strictures by CT.
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http://dx.doi.org/10.1007/s00464-021-08661-1DOI Listing
May 2022

Characterization of Functional Groups in Estuarine Dissolved Organic Matter by DNP-enhanced N and C Solid-State NMR.

Chemphyschem 2021 09 19;22(18):1907-1913. Epub 2021 Aug 19.

Univ. Lille, CNRS, Centrale Lille, Univ. Artois, UMR 8181 - UCCS - Unité de Catalyse et Chimie du Solide, 59000, Lille, France.

Estuaries are key ecosystems with unique biodiversity and are of high economic importance. Along the estuaries, variations in environmental parameters, such as salinity and light penetration, can modify the characteristics of dissolved organic matter (DOM). Nevertheless, there is still limited information about the atomic-level transformations of DOM in this ecosystem. Solid-state NMR spectroscopy provides unique insights into the nature of functional groups in DOM. A major limitation of this technique is its lack of sensivity, which results in experimental time of tens of hours for the acquisition of C NMR spectra and generally precludes the observation of N nuclei for DOM. We show here how the sensitivity of solid-state NMR experiments on DOM of Seine estuary can be enhanced using dynamic nuclear polarization (DNP) under magic-angle spinning. This technique allows the acquisition of C NMR spectra of these samples in few minutes, instead of hours for conventional solid-state NMR. Both conventional and DNP-enhanced C NMR spectra indicate that the C local environments in DOM are not strongly modified along the Seine estuary. Furthermore, the sensitivity gain provided by the DNP allows the detection of N NMR signal of DOM, in spite of the low nitrogen content. These spectra reveal that the majority of nitrogen is in the amide form in these DOM samples and show an increased disorder around these amide groups near the mouth of the Seine.
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http://dx.doi.org/10.1002/cphc.202100334DOI Listing
September 2021

Bidentate Disilicate Framework for Bis-Grafted Surface Species.

Chemistry 2021 Aug 29;27(47):12069-12077. Epub 2021 Jul 29.

National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba Central 5, 1-1-1 Higashi, Tsukuba, Ibaraki, 305-8565, Japan.

Recent advances in surface organometallic chemistry have enabled the detailed characterization of the surface species in single-site heterogeneous catalysts. However, the selective formation of bis-grafted surface species remains challenging because of the heterogeneity of the supporting surface. Herein, we introduce a metal complex bearing bidentate disilicate ligands, -OSi(O Bu) OSi(O Bu) O-, as a molecular precursor, which has a silicate framework adjacent to the metal (Pt) center. The grafting of the precursors on silica supports (MCM-41 and CARiACT Q10) proceeded through a substitution reaction on the silicon atoms of the disilicate ligand, which was verified by the detection of isobutene and BuOH as the elimination products, to selectively yield bis-grafted surface species. The chemical structure of the surface species was characterized by solid-state NMR, and the chemical shift values of the ancillary ligands and Pt nuclei suggested that the bidentate coordination sphere was maintained following grafting.
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http://dx.doi.org/10.1002/chem.202101927DOI Listing
August 2021

Transparent Organogel Films Showing Extremely Efficient and Durable Anti-Icing Performance.

ACS Appl Mater Interfaces 2021 Jun 13;13(24):28925-28937. Epub 2021 Jun 13.

Innovative Functional Materials Research Institute, National Institute of Advanced Industrial Science and Technology (AIST), 2266-98, Anagahora, Shimo-shidami, Moriyama, Nagoya 463-8560, Japan.

Accumulation of ice and snow on solid surfaces causes destructive problems in our daily life. Therefore, the development of functional coatings/surfaces that can effectively prevent ice/snow adhesion by natural forces, such as airflow, vibration, solar radiation, or gravity, is in high demand. In this study, transparent organogel films possessing negligible ice adhesion strength were successfully designed by a simple cross-linking of poly(dimethylsiloxane) (PDMS) in the presence of commercially available oils. Both the molecular weights (MWs) of the infusing oils and their contents in the PDMS matrices have proven to be key parameters for primarily determining the cross-linking density of PDMS matrices and syneresis/nonsyneresis behaviors of our samples, which closely reflected the final surface static/dynamic dewetting and anti-icing properties. By tuning only these two parameters, three different types of transparent organogel films, that is, nonsyneresis organogel (NSG), self-lubricating organogel (SLUG-I, infused with highly mobile oils), and SLUG-II (infused with viscous oils) films, were prepared. Among them, on the SLUG-I films, the lubricating oils were found to be continuously released from the PDMS matrices through syneresis for more than 1 year. Due to this unusual syneresis behavior, the ice adhesion strength became virtually zero, and this excellent anti-icing property also remained almost unchanged even after several cycles of icing/deicing testing. On the other hand, in the case of SLUG-II films, as the lubricated oil layers were too viscous, ice had trouble sliding off the surfaces by gravity. In contrast to these SLUG films, ice adhesion strength on NSG films was markedly decreased by increasing the amount of the infusing oils. In spite of NSG films having no distinct mobile oil layer, the ice adhesion strength reached its minimum of only about 5 kPa.
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http://dx.doi.org/10.1021/acsami.1c06815DOI Listing
June 2021

Analysis of circulating cell-free DNA after endoscopic ultrasound-guided fine needle aspiration in pancreatic ductal adenocarcinoma.

Pancreatology 2021 Apr 15. Epub 2021 Apr 15.

Department of Gastroenterology, Graduate School of Medicine, Chiba University, Chiba, Japan.

Background/objectives: Recently, increase in cell-free DNA (cfDNA) concentration or newly detected KRAS mutation after endoscopic ultrasound-guided fine needle aspiration (EUS-FNA) biopsy were reported to be related to the occurrence of new distant metastasis. In this study, we investigated whether cfDNA concentration increased with the release of tumor components into the blood after EUS-FNA and whether its increase was related to prognosis.

Methods: Sixty-eight patients underwent EUS-FNA and were pathologically confirmed as having pancreatic ductal adenocarcinoma (PDAC). We measured plasma cfDNA concentration and the copy number of KRAS mutation in 68 patients and circulating tumor cells in 8 before and after EUS-FNA.

Results: The average cfDNA concentration after EUS-FNA (672.5 ± 919.6 ng/mL) was significantly higher than that before EUS-FNA (527.7 ± 827.3 ng/mL) (P < 0.001). KRAS mutation in plasma was detected in 8 patients (11.8%), however a significant increase in cfDNA concentration after EUS-FNA was not related to the change in KRAS-mutant copy number. Minimal increase in circulating tumor cells was observed in 3 of 8 patients. New distant metastasis was observed within 286 days to initial metastasis detection in 6 of 12 patients with ≥2-fold increase in cfDNA concentration and 26 of 56 patients with <2-fold increase within 185 days. In 32 patients who underwent surgery, ≥2-fold increase in cfDNA did not affect early recurrence.

Conclusions: The increase in cfDNA concentration after EUS-FNA was not caused by tumor cell components released into blood vessels. Hence, the risk of seeding via the blood stream after EUS-FNA may need not be considered.
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http://dx.doi.org/10.1016/j.pan.2021.04.001DOI Listing
April 2021

Analysis of the possible cytogenetic mechanism for overcoming hybrid lethality in an interspecific cross between Nicotiana suaveolens and Nicotiana tabacum.

Sci Rep 2021 04 9;11(1):7812. Epub 2021 Apr 9.

Graduate School of Agricultural Science, Tokyo University of Agriculture and Technology, Tokyo, 183-0054, Japan.

Hybrid lethality is a type of reproductive isolation in which hybrids die before maturation, due to the interaction between the two causative genes derived from each of the hybrid parents. The interspecific hybrid of Nicotiana suaveolens × Nicotiana tabacum is a model plant used in studies on hybrid lethality. While most of the progeny produced from such a cross die, some individuals grow normally and mature. Separately, a technique for producing mature hybrids by artificial culture has been developed. However, the mechanism by which hybrids overcome lethality, either spontaneously or by artificial culture, remains unclear. In the present study, we found that some hybrids that overcome lethality, either spontaneously or by artificial culture, lack the distal part of the Q chromosome, a region that includes the gene responsible for lethality. Quantitative polymerase chain reaction results suggested that the distal deletion of the Q chromosome, detected in some hybrid seedlings that overcome lethality, is caused by reciprocal translocations between homoeologous chromosomes. The results showed that chromosomal instability during meiosis in amphidiploid N. tabacum as well as during artificial culturing of hybrid seedlings is involved in overcoming hybrid lethality in interspecific crosses of the genus Nicotiana.
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http://dx.doi.org/10.1038/s41598-021-87242-7DOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC8035154PMC
April 2021

Percutaneous Two-Dimensional Shear Wave Elastography for Diagnosis of Pancreatic Tumor.

Diagnostics (Basel) 2021 Mar 11;11(3). Epub 2021 Mar 11.

Department of Gastroenterology, Chiba University Graduate School of Medicine, 1-8-1 Inohan, Chuo-ku Chiba City 260-8670, Japan.

Background: To investigate the efficacy of two-dimensional shear wave elastography (2D-SWE) for the diagnosis of pancreatic mass lesions.

Methods: This ethics committee-approved cross-sectional study included 52 patients with histologically-proven pancreatic tumors (pancreatic ductal adenocarcinoma (PDAC), 36; tumor-forming pancreatitis (TFP), 15; neuroendocrine tumor, 1) and 33 control subjects. The 2D-SWE was performed for the tumor/non-tumor tissues, and SWE-mapping patterns and propagation quality were assessed.

Results: Three mapping patterns were detected based on the size and distribution of the coloring areas. Pattern A (whole coloring) was detected in all non-tumor tissues and TFP, whereas pattern C (multiple small coloring spots) was detected in PDAC only. Pattern B (partial coloring with smaller spots) was detected in other lesions. The specificity and positive predictive value of pattern A for non-PDAC and those of pattern C for PDAC were 100%. The SWE value was higher in tumor lesions than in the non-tumor tissues (38.1 vs. 9.8 kPa; < 0.001) in patients with PDAC. The SWE value in the non-tumor lesion was higher in patients with PDAC than in control (9.8 vs. 7.5 kPa; < 0.001).

Conclusions: 2D-SWE may play a role as a novel diagnostic tool for PDAC to detect a specific mapping pattern with quantitative assessment.
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http://dx.doi.org/10.3390/diagnostics11030498DOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC8001884PMC
March 2021

Efficient transfer of DNP-enhanced H magnetization to half-integer quadrupolar nuclei in solids at moderate spinning rate.

Magn Reson Chem 2021 Sep 14;59(9-10):920-939. Epub 2021 Jan 14.

Univ. Lille, CNRS, Centrale Lille, Univ. Artois, UMR 8181-UCCS-Unité de Catalyse et de Chimie du Solide, Lille, France.

We show herein how the proton magnetization enhanced by dynamic nuclear polarization (DNP) can be efficiently transferred at moderate magic-angle spinning (MAS) frequencies to half-integer quadrupolar nuclei, S ≥ 3/2, using the Dipolar-mediated Refocused Insensitive Nuclei Enhanced by Polarization Transfer (D-RINEPT) technique, in which a symmetry-based recoupling scheme built from adiabatic inversion H pulses reintroduces the H-S dipolar couplings, while suppressing the H- H ones. The use of adiabatic pulses also improves the robustness to offsets and radiofrequency (rf)-field inhomogeneity. Furthermore, the efficiency of the polarization transfer is further improved by using H composite pulses and continuous-wave irradiations between the recoupling blocks, as well as by manipulating the S satellite transitions during the first recoupling block. Furthermore, in the case of large H-S dipolar couplings, the D-RINEPT variant with two pulses on the quadrupolar channel results in an improved transfer efficiency. We compare here the performances of this new adiabatic scheme with those of its parent version with single π pulses, as well as with those of PRESTO and CPMAS transfers. This comparison is performed using simulations as well as DNP-enhanced Al, Mo, and O NMR experiments on isotopically unmodified γ-alumina, hydrated titania-supported MoO , Mg(OH) , and l-histidine·HCl·H O. The introduced RINEPT method outperforms the existing methods, both in terms of efficiency and robustness to rf-field inhomogeneity and offset.
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http://dx.doi.org/10.1002/mrc.5121DOI Listing
September 2021

Observation of Low-γ Quadrupolar Nuclei by Surface-Enhanced NMR Spectroscopy.

J Am Chem Soc 2020 06 4;142(24):10659-10672. Epub 2020 Jun 4.

Univ. Lille, CNRS, Centrale Lille, Univ. Artois, UMR 8181, UCCS - Unité de Catalyse et de Chimie du Solide, F-59000 Lille, France.

We introduce a novel NMR approach that extends the capabilities of indirect dynamic nuclear polarization (DNP) under magic-angle spinning to probe the local environment of half-integer spin quadrupolar nuclei. Compared to cross-polarization, this novel method based on the refocused INEPT scheme with adiabatic dipolar recoupling is easier to optimize and does not distort the quadrupolar line shapes. Furthermore, the use of this technique, instead of the PRESTO (Phase-shifted Recoupling Effects a Smooth Transfer of Order) scheme or direct DNP, greatly improves the sensitivity of DNP-NMR for the detection of quadrupolar isotopes with small dipolar couplings to protons, including notably those located in the subsurface of inorganic materials or with low gyromagnetic ratio (γ). This technique has been applied to identify the atomic-level structure of Brønsted acid sites of hydrated titania-supported MoO, MoO/TiO, a widely used heterogeneous catalyst. The spectra of protonated and unprotonated O sites, acquired in natural abundance, indicate the presence of various oxomolybdate species as well as HOMo and HOMo Brønsted acid sites. The enhanced sensitivity of this new method has also enabled the acquisition of the first DNP-enhanced spectra of Mo and Ti low-γ quadrupolar isotopes. This possibility has been demonstrated by detecting the signals of these nuclei near the surface of MoO/TiO. This technique has allowed the observation of Ti surface sites, which are absent from the bulk region of TiO. Furthermore, both Mo and Ti DNP spectra have shown an increased structural disorder of TiO and MoO phases near the surface of the particles and notably the preferential location of the amorphous TiO phase at the surface of the particles. The proposed polarization transfer is also employed to acquire the first DNP-enhanced spectrum of Zn, another low-γ quadrupolar isotope. This possibility is demonstrated for Al-doped ZnO nanoparticles used in optoelectronic devices. The obtained O, Al, and Zn DNP-NMR data prove that the surface region of these nanoparticles contains ZnO phase as well as secondary phases, such as α-AlO and partially inverse ZnAlO spinel.
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http://dx.doi.org/10.1021/jacs.9b13838DOI Listing
June 2020

Ultra-Narrow Depletion Layers in a Hematite Mesocrystal-Based Photoanode for Boosting Multihole Water Oxidation.

Angew Chem Int Ed Engl 2020 Jun 30;59(23):9047-9054. Epub 2020 Apr 30.

Molecular Photoscience Research Center, Kobe University, 1-1 Rokkodai-cho, Nada-ku, Kobe, 657-8501, Japan.

Significant charge recombination that is difficult to suppress limits the practical applications of hematite (α-Fe O ) for photoelectrochemical water splitting. In this study, Ti-modified hematite mesocrystal superstructures assembled from highly oriented tiny nanoparticle (NP) subunits with sizes of ca. 5 nm were developed to achieve the highest photocurrent density (4.3 mA cm at 1.23 V vs. RHE) ever reported for hematite-based photoanodes under back illumination. Owing to rich interfacial oxygen vacancies yielding an exceedingly high carrier density of 4.1×10  cm for super bulk conductivity in the electrode and a large proportion of ultra-narrow depletion layers (<1 nm) inside the mesoporous film for significantly improved hole collection efficiency, a boosting of multihole water oxidation with very low activation energy (E =44 meV) was realized.
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http://dx.doi.org/10.1002/anie.202001919DOI Listing
June 2020

Orientation of Ligand Field for Dangling Manganese in Photosynthetic Oxygen-Evolving Complex of Photosystem II.

J Phys Chem B 2020 01 23;124(1):128-133. Epub 2019 Dec 23.

Division of Material Science, Graduate School of Science , Nagoya University , Furo-cho , Chikusa-ku, 464-8602 Nagoya , Aichi , Japan.

The spin structure in the S state and the crystal structure of the manganese cluster of the oxygen-evolving complex of plant photosystem II were combined by the quantitative evaluation of the magnetic anisotropy of the = 4 signal. The -values of 3.93 and 4.13 were obtained for the = 4 signal in the directions parallel and perpendicular to the membrane normal, respectively. The peak-to-peak separations were 270 and 420 G for the parallel and perpendicular orientations to the membrane, respectively. By comparison with the crystal structure, the -axis of the zero-field splitting was ascribed to the direction of the dangling Mn connecting water oxygen, Mn4-O(W1), in the manganese cluster. The results give the first experimental evidence that the valence of the dangling Mn is Mn(III) in the S high-spin state. We showed that the strong exchange coupling of Mn4 to Mn3 was required for = 4.1 spin state in the four-spin couplings, estimated as > ∼|-30 cm|, indicating that the present closed cubane model in quantum mechanics/molecular mechanics (QM/MM) calculation cannot explain the = 4.1 spin structure. The onsite zero-field splitting of the dangling Mn was evaluated as -2.3 cm under the strong antiferromagnetic couplings (-50 cm) with the dangling Mn to the cubane frame in the four coupled spin state. From the viewpoint of the arrangement of the Mn valences in the cluster, a closed cubane model is effective, but without a large structural deviation from the S state crystal structure.
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http://dx.doi.org/10.1021/acs.jpcb.9b10817DOI Listing
January 2020

Interfacial oxygen vacancies yielding long-lived holes in hematite mesocrystal-based photoanodes.

Nat Commun 2019 10 23;10(1):4832. Epub 2019 Oct 23.

Department of Chemistry, Graduate School of Science, Kobe University, 1-1 Rokkodai-cho, Nada-ku, Kobe, 657-8501, Japan.

Hematite (α-FeO) is one of the most promising candidates as a photoanode materials for solar water splitting. Owing to the difficulty in suppressing the significant charge recombination, however, the photoelectrochemical (PEC) conversion efficiency of hematite is still far below the theoretical limit. Here we report thick hematite films (∼1500 nm) constructed by highly ordered and intimately attached hematite mesocrystals (MCs) for highly efficient PEC water oxidation. Due to the formation of abundant interfacial oxygen vacancies yielding a high carrier density of ∼10 cm and the resulting extremely large proportion of depletion regions with short depletion widths (<10 nm) in hierarchical structures, charge separation and collection efficiencies could be markedly improved. Moreover, it was found that long-lived charges are generated via excitation by shorter wavelength light (below ∼500 nm), thus enabling long-range hole transfer through the MC network to drive high efficiency of light-to-energy conversion under back illumination.
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http://dx.doi.org/10.1038/s41467-019-12581-zDOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC6811569PMC
October 2019

Controlled Orientations of Neighboring Tetracene Units by Mixed Self-Assembled Monolayers on Gold Nanoclusters for High-Yield and Long-Lived Triplet Excited States through Singlet Fission.

J Am Chem Soc 2019 Sep 6;141(37):14720-14727. Epub 2019 Sep 6.

Department of Chemistry, Faculty of Science and Technology , Keio University , 3-14-1 Hiyoshi , Kohoku-ku, Yokohama , Kanagawa 223-8522 , Japan.

Although tetracene (Tc) is well-known as a good candidate for singlet fission (SF), the number of high-yield and long-lived triplet excited states through SF is extremely limited because of the relative acceleration of the reverse triplet-triplet annihilation (TTA) considering the energy matching between a singlet and two triplet states. Systematic control of electronic interactions between two neighboring units using conventional covalent linkages and molecular assembly methods to optimize these kinetic processes is quite difficult because of the complicated synthesis and random orientations. In this study, we propose a novel supramolecular strategy utilizing mixed self-assembled monolayers (SAMs) with two different chain lengths. Specifically, mixed Tc-SAMs on gold nanoclusters, which are prepared using Tc-modified heterodisulfides with two different chain lengths, attain high-yield SF (Φ ≈ 90%) and individual triplet yields (Φ ≈ 160%). The obtained Φ is the highest value among Tc derivatives in homogeneous solution to the best of our knowledge.
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http://dx.doi.org/10.1021/jacs.9b06567DOI Listing
September 2019

Identifying triplet pathways in dilute pentacene films.

Nat Commun 2018 10 11;9(1):4222. Epub 2018 Oct 11.

Institute of Structural and Molecular Biology and London Centre for Nanotechnology, University College London, Gower Street, London, WC1E 6BT, UK.

Building efficient triplet-harvesting layers for photovoltaic applications requires a deep understanding of the microscopic properties of the components involved and their dynamics. Singlet fission is a particularly appealing mechanism as it generates two excitons from a single photon. However, the pathways of the coupled triplets into free species, and their dependence on the intermolecular geometry, has not been fully explored. In this work, we produce highly ordered dilute pentacene films with distinct parallel and herringbone dimers and aggregates. Using electron paramagnetic resonance spectroscopy, we provide compelling evidence for the formation of distinct quintet excitons in ambient conditions, with intrinsically distinctive electronic and kinetic properties. We find that the ability of quintets to separate into free triplets is promoted in the parallel dimers and this provides molecular design rules to control the triplets, favouring either enhanced photovoltaic efficiency (parallel) or strongly bound pairs that could be exploited for logic applications (herringbone).
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http://dx.doi.org/10.1038/s41467-018-06330-xDOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC6181988PMC
October 2018

Singlet-Fission-Born Quintet State: Sublevel Selections and Trapping by Multiexciton Thermodynamics.

J Phys Chem Lett 2018 Oct 26;9(19):5855-5861. Epub 2018 Sep 26.

Molecular Photoscience Research Center , Kobe University , 1-1 Rokkodai-cho, Nada-ku , Kobe , Hyogo 657-8501 , Japan.

Singlet fission (SF) is expected to exceed the theoretical limit of the solar cell efficiency. Quintet (Q) state generation in triplet-triplet pair is essential for preventing the unwanted loss of SF-born multiexciton through singlet channels, although little is known on the primary multiexciton spin dynamics following the intermolecular SF. In this study, time-resolved EPR revealed the intermolecular multiexciton dynamics, energetics and geometries in aggregated 6,13-bis(triisopropylsilylethynyl)pentacene and 2-phenyl-6,11-bis(triisopropylsilylethynyl)tetracene in diluted frozen solution. We have demonstrated sublevel selective generations of excited quintet states (|Q⟩, |Q⟩ and |Q⟩) by singlet-quintet (SQ) mixings during triplet-exciton diffusions within geminate multiexcitons. The present fundamental characteristics of the quintet generations shows strong impact of coexistence of molecularly ordered "hot spot" and disordered regions for exergonic SQ mixings driven by entropy, thereby paving a new avenue for rational designs of organic devices with controlled multiexciton dynamics by optimizing film morphologies.
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http://dx.doi.org/10.1021/acs.jpclett.8b02396DOI Listing
October 2018

N overtone nuclear magnetic resonance of rotating solids.

J Chem Phys 2018 Aug;149(6):064201

Shanghai Key Laboratory of Magnetic Resonance, School of Physics and Materials Science, East China Normal University, Shanghai 200062, China.

By irradiating and observing at twice the N Larmor frequency, overtone (OT) nuclear magnetic resonance (NMR) is capable of obtaining N spectra without first-order quadrupolar broadening. Direct excitation and detection of the usually "forbidden" double-quantum transition is mediated by the perturbation from the large quadrupole interaction to the spin states quantized by the Zeeman interaction. A recent study [L. A. O'Dell and C. I. Ratcliffe, Chem. Phys. Lett. , 168 (2011)] has shown that N NMR under magic-angle spinning (MAS) can yield high-resolution spectra with typical second-order quadrupolar line shapes allowing the measurement of N chemical shift and quadrupolar coupling parameters. This article has also shown that under MAS the main N peak is shifted by twice the sample spinning frequency with respect to its static position. We present the theory of N NMR of static or rotating samples and the physical picture of the intriguing spinning-induced shift in the second case. We use perturbation theory for the case of static samples and Floquet theory for rotating samples. In both cases, the results can be described by a so-called OT parameter that scales down the N radio-frequency () excitation and signal detection. This OT parameter shows that the components of the field, which are transverse and longitudinal with respect to the magnetic field, are both effective for N excitation and signal detection. In the case of MAS at angular frequency , the superposition of the excitation and detection components in the OT parameter makes either the +2 or -2 term the dominant N signal, depending on the sense of sample spinning with respect to the magnetic field. This leads to an apparent N signal shifted at twice the spinning frequency. The features of N NMR spectra for both static and rotating samples are illustrated with simulations. The spinning induced shift and its dependence on the spinning direction are confirmed experimentally by reversing the spinning direction and the field of the 36 T series-connected hybrid magnet at the US National High Magnetic Field Laboratory.
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http://dx.doi.org/10.1063/1.5044653DOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC8808743PMC
August 2018

Observation of proximities between spin-1/2 and quadrupolar nuclei in solids: Improved robustness to chemical shielding using adiabatic symmetry-based recoupling.

Solid State Nucl Magn Reson 2018 10 20;94:7-19. Epub 2018 Jul 20.

Univ. Lille, CNRS-8181, UCCS-Unit of Catalysis and Chemistry of Solids, F-59000, Lille, France; Institut Universitaire de France, 1 rue Descartes, F-75231, Paris, France. Electronic address:

We introduce a novel heteronuclear dipolar recoupling based on the R2 symmetry, which uses the tanh/tan (tt) shaped pulse as a basic inversion element and is denoted R2(tt). Using first-order average Hamiltonian theory, we show that this sequence is non-γ-encoded and that it reintroduces the |m| = 1 spatial component of the Chemical Shift Anisotropy (CSA) of the irradiated isotope and its heteronuclear dipolar interactions. Using numerical simulations and one-dimensional (1D) Al-{P} through-space D-HMQC (Dipolar Heteronuclear Multiple-Quantum Correlation) experiments on VPI-5, we compare the performances of this recoupling to those of other non-γ-encoded |m| = 1 heteronuclear recoupling schemes: REDOR (Rotational-Echo DOuble Resonance), SFAM (Simultaneous Frequency and Amplitude Modulation) and R4(tt). Such comparison indicates that the R2(tt) scheme is more robust to CSA, offset and radiofrequency field inhomogeneities than the other schemes. We take advantage of the high robustness of R2(tt) to CSA and offset to demonstrate the possibility to correlate the signals of Pb isotope with those of neighboring half-integer spin quadrupolar nuclei. Such approach is demonstrated experimentally by acquiring B-{Pb} D-HMQC 2D spectra of PbO(BO) crystalline powder.
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http://dx.doi.org/10.1016/j.ssnmr.2018.07.001DOI Listing
October 2018

Multiexciton Dynamics Depending on Intramolecular Orientations in Pentacene Dimers: Recombination and Dissociation of Correlated Triplet Pairs.

J Phys Chem Lett 2018 Jun 6;9(12):3354-3360. Epub 2018 Jun 6.

Department of Chemistry , Faculty of Science and Technology, Keio University , Yokohama 223-8522 , Japan.

Pentacene dimers bridged by a phenylene at ortho and meta positions [denoted as o-(Pc) and m-(Pc)] were synthesized to examine intramolecular orientation-dependent multiexciton dynamics, especially focusing on singlet fission (SF) and recombination from correlated triplet pairs [(TT)]. Absorption and electrochemical measurements indicated strong intramolecular couplings of o-(Pc) relative to m-(Pc). Femtosecond and nanosecond TA measurements successfully demonstrated efficient SF in both dimers. In contrast, the dissociation process from the (TT) to the individual triplets [(2 × T)] was clearly observed in m-(Pc), which is in sharp contrast to a major recombination process in o-(Pc). Time-resolved electron spin resonance (TR-ESR) measurements demonstrated that the recombination and dissociation proceed from the quintet state of (TT) in m-(Pc). The rate constant of the SF was 2 orders of magnitude greater in o-(Pc) than that in m-(Pc) and was rationalized by enhanced electronic coupling between adjacent HOMOs of the Pc units.
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http://dx.doi.org/10.1021/acs.jpclett.8b01184DOI Listing
June 2018

Magnetic structure of manganese cluster in photosystem II investigated by electron paramagnetic resonance.

Biophys Physicobiol 2018 6;15:45-50. Epub 2018 Feb 6.

Division of Material Science (Physics), Graduate School of Science, Nagoya University, Nagoya, Aichi 464-8602, Japan.

The electronic structure of manganese (Mn) cluster in photosystem II was investigated by electron paramagnetic resonance (EPR) spectroscopy. In order to determine the spin density distribution in magnetically coupled Mn in the S state Mn cluster, pulsed electron-electron double resonance (PELDOR) measurement was performed. The local environment of the Mn cluster was investigated by electron-nuclear double resonance (ENDOR). Using spin projections determined by PELDOR, ENDOR signals were assigned to the water molecules ligated to the Mn cluster. The location of a high-affinity Mn site in apo-photosystem II, which is the initial site of photoactivation of the Mn cluster, was determined by PELDOR.
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http://dx.doi.org/10.2142/biophysico.15.0_45DOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC5873039PMC
February 2018

Dimeric Structure of the Blue Light Sensor Protein Photozipper in the Active State.

Biochemistry 2018 02 21;57(5):494-497. Epub 2017 Dec 21.

Division of Material Science, Graduate School of Science, Nagoya University , Chikusa-ku, Furo-cho, Nagoya 464-8602, Japan.

The light oxygen voltage-sensing (LOV) domain plays a crucial role in blue light (BL) sensing in plants and microorganisms. LOV domains are usually associated with the effector domains and regulate the activities of effector domains in a BL-dependent manner. Photozipper (PZ) is monomeric in the dark state. BL induces reversible dimerization of PZ and subsequently increases its affinity for the target DNA sequence. In this study, we report the analyses of PZ by pulsed electron-electron double resonance (PELDOR). The neutral flavin radical was formed by BL illumination in the presence of dithiothreitol in the LOV-C254S (without the bZIP domain) and PZ-C254S mutants, where the cysteine residue responsible for adduct formation was replaced with serine. The magnetic dipole interactions of 3 MHz between the neutral radicals were detected in both LOV-C254S and PZ-C254S, indicating that these mutants are dimeric in the radical state. The PELDOR simulation showed that the distance between the radical pair is close to that estimated from the dimeric crystal structure in the "light state" [Heintz, U., and Schlichting, I. (2016) eLife 5, e11860], suggesting that in the radical state, LOV domains in PZ-C254S form a dimer similar to that of LOV-C254S, which lacks the bZIP domain.
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http://dx.doi.org/10.1021/acs.biochem.7b01045DOI Listing
February 2018

Frequency of Acute Kidney Injury Caused by Tazobactam/Piperacillin in Patients with Pneumonia and Chronic Kidney Disease: A Retrospective Observational Study.

Yakugaku Zasshi 2017 ;137(9):1129-1136

Department of Clinical Pharmacy School of Pharmaceutical Sciences, Kobe Gakuin University.

 Tazobactam/piperacillin (TAZ/PIPC) is a combination antibiotic frequently used to treat pneumonia. It has recently been reported that TAZ/PIPC worsens renal function in patients with existing renal impairment. Creatinine clearance is generally between 10 and 40 mL/min in Japanese patients, so TAZ/PIPC is given at a dose of 2.25 g three times daily or 4.5 g twice daily. If pneumonia is severe or intractable, the dose frequency may be increased to 2.25 g four times daily and 4.5 g three times daily. We examined the effect of these different dosing regimens on renal function. We studied a cohort of 57 patients with impaired renal function hospitalized with pneumonia and treated with TAZ/PIPC between January 2015 and November 2016. Patients were classified into four groups according to TAZ/PIPC dose: 2.25 g three times daily (Group A); 2.25 g four times daily (B); 4.5 g twice daily (C) and 4.5 g three times daily (D). We examined the frequency of acute kidney injury (AKI) and treatment effectiveness. In Groups A, B, C and D, AKI occurred in 5.6%, 0.0%, 25.0% and 38.5% of patient. In groups C and D, hydration and dose reduction were required to address early signs of impending AKI. Our findings suggest that the higher TAZ/PIPC dose of 4.5 g was responsible for the decline in renal function, even if the dose frequency was reduced.
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http://dx.doi.org/10.1248/yakushi.17-00002DOI Listing
November 2017
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