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Xiu-Jun Wu, Xin Huang, Hai-Yan Shi, Xing-Kai Chen, Qian Dong, Guo-Xiang Hao, Yan Li, Yi Zheng, Wei Zhao
A rapid, accurate and specific high-performance liquid chromatographic -tandem mass spectrometry method has been validated for the simultaneous determination of cefoperazone and sulbactam in a small volume sample for children. A Shim-pack XR-ODS C18 column with gradient elution of water (0.1% formic acid) and acetonitrile (0.1% formic acid) solution was used for separation at a flow rate of 0.3 mL/min. The calibration curves of two analytes in serum showed excellent linearity over the concentration ranges of 0...
November 17, 2017: Biomedical Chromatography: BMC
Zhi-Chao Liao, Xin Jiang, Wen-Jing Tian, Ting Lin, Hai-Feng Chen
The compounds were isolated and purified by HP20 macroporous adsorption resin, ODS, silica gel, and Sephadex LH-20 column chromatography, as well as semi-preparative HPLC chromatography from the 80% ethanol extract of the root of Angelica decursiva, and their structures were identified based on their physiochemical properties and spectroscopic data. Twelve compounds were structures were identified as (9R,10R)-9-acetoxy-8,8-dimethyl-9,10-dihydro-2H,8H-benzo[1,2-b:3,4-b']dipyran-2-one-10-yl ester (1), bakuchicin (2), (3', S,4'S)-disenecioyloxy-3',4'-dihydroseselin (3), (3'R,4'R)-3'-angeloyloxy-4'-senecioyloxy-3',4'-dihydroseselincalipteryxin (4), (+)-8,9-dihydro-8-(2-hydroxypropan-2-yl)-2-oxo-2H-furo[2,3h]chromen-9-yl-3-methylbut-2-enoate (5), libanoridin (6), selinidin (7), suberosin (8), crocatone (9), peujaponisinol B (10), peujaponisinol A (11), and ostenol (12), respectively...
August 2017: Zhongguo Zhong Yao za Zhi, Zhongguo Zhongyao Zazhi, China Journal of Chinese Materia Medica
Miho Yamada, Xiao-Pen Lee, Masaya Fujishiro, Ken Iseri, Makoto Watanabe, Hiroshi Sakamaki, Naoki Uchida, Takaaki Matsuyama, Takeshi Kumazawa, Haruo Takahashi, Akira Ishii, Keizo Sato
A highly sensitive method was developed for the analysis of alendronate in human plasma and dialysate using MonoSpin™ SAX(®) extraction and metal-free high-performance liquid chromatography (HPLC)-tandem mass spectrometry (MS/MS) following methylation with trimethylsilyldiazomethane. The chromatographic separation of the derivatives for alendronate and alendronate-d6 was achieved on an L-column2 ODS metal-free column (50 mm  ×  2 mm i.d., particle size 3 µm) with a linear gradient elution system composed of 10 mM ammonium acetate (pH 6...
November 6, 2017: Legal Medicine
Xiao Shu, Qing Dai, Tong Wu, Ian R Bothwell, Yanan Yue, Zezhou Zhang, Jie Cao, Qili Fei, Minkui Luo, Chuan He, Jianzhao Liu
RNA labeling is crucial for the study of RNA structure and metabolism. Herein we report N(6)-allyladenosine (a(6)A) as a new small molecule for RNA labeling through both metabolic and enzyme-assisted manners. a(6)A behaves like A and can be metabolically incorporated into newly synthesized RNAs inside mammalian cells. We also show that human RNA N(6)-methyladenosine (m(6)A) methyltransferases METTL3/METTL14 can work with a synthetic cofactor, namely allyl-SAM (S-adenosyl methionine with methyl replaced by allyl) in order to site-specifically install an allyl group to the N(6)-position of A within specific sequence to generate a(6)A-labeled RNAs...
November 15, 2017: Journal of the American Chemical Society
Andrea Lastovkova, Melanie Carder, Hans Martin Rasmussen, Lars Sjoberg, Gerda J de Groene, Riitta Sauni, Jiri Vevoda, Sarka Vevodova, Gerard Lasfargues, Magnus Svartengren, Marek Varga, Claudio Colossio, Daniela Pelclova
The risk of psychological disorders influencing the health of workers increases in accordance with growing requirements on employees across various professions. This study aimed to compare approaches to the burnout syndrome in European countries. A questionnaire focusing on stress-related occupational diseases was distributed to national experts of 28 European Union countries. A total of 23 countries responded. In 9 countries (Denmark, Estonia, France, Hungary, Latvia, Netherlands, Portugal, Slovakia and Sweden) burnout syndrome may be acknowledged as an occupational disease...
November 3, 2017: Industrial Health
Yuzhong Wang, Hunter P Hickox, Yaoming Xie, Pingrong Wei, Henry F Schaefer, Gregory H Robinson
Reaction of thiolate 1 with carbene-stabilized diiodo-bis-silylene (2) (in a 2:1 ratio) in THF unexpectedly gives both the first five-membered, sulfur-containing, zwitterionic silylene ring (3) via insertion of the "Si(I)2" unit of 2 into the olefinic C-H bond of the imidazole ring of 1 and four-membered cyclic silylene (4) via insertion of a silicon(I) atom of 2 into the Cphenyl-N bond of the carbene ligand. The parallel reaction in toluene only gives 3 as the major product. The nature of the bonding in isomeric 3 and 4 was probed by experimental and theoretical methods...
November 15, 2017: Journal of the American Chemical Society
Ge Han, Hao Xu, Wei Gong, Xin Ma, Ailin Liang
The increase of greenhouse gas is one of the most important factors leading to global climate change. Differential absorption lidar (DIAL) is considered to be the tool with the most potential to measure CO2 remotely. However, it is difficult to obtain accurate CO2 retrievals and determine carbon fluxes with the traditional dual-wavelength differential absorption inversion method, which is characterized by a low signal-to-noise ratio (SNR). Therefore, a multi-wavelength differential absorption inversion framework is proposed in this work...
October 20, 2017: Applied Optics
Yue-Mei Chen, Nan-Kai Cao, Peng-Fei Tu, Yong Jiang
The open silica gel, ODS, and Sephadex LH-20 column chromatography, along with the semi-preparative HPLC was used to isolate and purify the chemical constituents from Murraya euchrestifolia. The structures of the isolates were elucidated by their physiochemical properties, NMR, and MS spectroscopic data, as well as comparison with literature data. Eighteen compounds were isolated from the CH2Cl2 fraction of the 95% aqueous EtOH extract of M. euchrestifolia, and their structures were identified as sakuranetin (1), eriodictyol-7,4'-dimethyl ether (2), isosakuranetin (3), 5-hydroxy-7,4'-dimethoxyflavanone (4), eriodictyol-7-methyl ether (5), lichexanthon (6), 5,6,7-trimethoxycoumarin (7), 5-hydroxy-6,8-dimethoxycoumarin (8), 8-hydroxy-6-methoxy-3-n-pentylisocoumarin (9), ethyl caffeate (10), 4-hydroxy-3,5- dimethoxycinnamic acid ethyl ester (11), methyl 3-(5'-hydroxyprenyl)-coumarate (12), (E)-coniferol (13), β-hydroxypropiovanillone (14), 3-hydroxy-7,8-didehydro-β-ionone (15), 3β-hydroxy-5α, 6α-epoxy-7-megastigmen-9-one (16), grasshopper ketone (17), and 4-hydroxy-3,5-dimethoxybenzaldehyde (18)...
May 2017: Zhongguo Zhong Yao za Zhi, Zhongguo Zhongyao Zazhi, China Journal of Chinese Materia Medica
Xian-Qiang Che, Shao-Ping Li, Jing Zhao
A new triterpenoid and 18 analogues were isolated from the water extract of Ganoderma lucidum by column chromatographic techniques, including silica gel, ODS, Sephadex LH-20, and HPLC. The new compound was elucidated as 2β-acetoxy-3β,25-dihydroxy-7,11,15-trioxo-lanost-8-en-26-oic acid on the basis of analyses of extensive spectroscopic data and its physicochemical properties. Comparison of NMR data with those reported in literature, the known analogues were determined as ganoderic acid H (2), 12β-acetoxy-3β,7β-dihydroxy-11,15,23-trioxo-lanost-8,16-dien-26-oic acid (3), ganoderenic acid D (4),ganoderic acid C1 (5),ganoderic acid G (6),3β,7β-dihydroxy-11,15,23-trioxo-lanost-8,16-dien-26-oic acid (7),ganoderic acid B (8),ganoderic acid C6 (9),3β,15α-dihydroxy-7,11,23-trioxo-lanost-8,16-dien-26-oic acid (10),ganoderic acid A (11),ganolucidic acid A (12),lucidenic acid E2 (13),lucidenic acid N (14),lucidenic acid P (15), lucidenic acid B (16),lucidenic acid A (17),lucidenic acid C (18),and lucidenic acid L (19), respectively...
May 2017: Zhongguo Zhong Yao za Zhi, Zhongguo Zhongyao Zazhi, China Journal of Chinese Materia Medica
Naoki Yoshioka, Hitoshi Ouchi, Toshiyuki Kan, Masashi Yoshida, Motoyuki Nomura
A rapid LC-MS method was developed for determination of acromelic acids A and B, which are toxic constituents of Paralepistopsis acromelalga (=Clitocybe acromelalga), in mushroom samples. Acromelic acids were extracted twice with 50% methanol and the extract was passed through a syringe filter, and then analyzed by LC-MS. The LC separation was performed on a multi-mode ODS column. The recoveries of acromelic acids A and B spiked into blank mushroom samples at 2.5 μg/g were 93 and 74%, respectively. This method was applied to the remaining mushroom sample from a food poisoning case...
2017: Shokuhin Eiseigaku Zasshi. Journal of the Food Hygienic Society of Japan
Shaima M Almasry, Eman M Habib, Rasha A Elmansy, Zeinab A Hassan
In this study, we addressed the potential relationship between prominin-1 (prom1) and vascular endothelial growth factor (VEGFA) in diabetes-induced retinopathy. In total, we examined 28 retinas from 14 rats with streptozotocin-induced diabetes and 30 retinas from 15 untreated control rats. ELISA was used to measure the level of prom1 and VEGFA in retinal tissue homogenates. Immunohistochemical techniques were used with antibodies directed against prom1, VEGFA, and CASP-3. After 180 days of diabetes induction, we performed light and electron microscopy studies on rat eyes to evaluate histopathological changes and to estimate the de novo metric "Diabetic Retinopathy Histopathological Index" (DRHI)...
October 1, 2017: Journal of Histochemistry and Cytochemistry: Official Journal of the Histochemistry Society
Xian-Jie Ma, Bao-Song Cui, Shao-Wei Han, Shuai Li
Eighteen compounds were isolated from the EtOAc soluble fraction of Bletilla striata by various chromatographic techniques, such as silica gel, ODS, Sephadex LH-20, RP-HPLC. Their structures were identified by spectroscopic methods and physicochemical properties, as 5-hydroxy-2-(p-hydroxybenzyl)- 3- methoxybibenzyl(1), shancigusins B(2), shanciguol(3),arundinan(4), 3',5-dihydroxy-2,4-di(p-hydroxybenzyl)-3-methoxybibenzyl(5), arundin(6), 3,3'-dihydroxy-2-(p-hydroxybenzyl)-5-methoxybibenzyl(7), 3, 3'-dihydroxy-2', 6'-bis(p-hydroxybenzyl)-5-methoxybibenzyl(8), 7-hydroxy-2,4-dimethoxyphenanthrene(9), bleformin B(10),nudol(11), 3,7-dihydroxy-2, 4-dimethoxyphenanthrene(12), 2, 7-dihydroxy-4-methoxy-9,10-dihydrophenathrene(13), bleformin D(14), 4,4'-dimethoxy-9,10-dyhydro-[6,1'-biphenanthrene]-2,2',7,7'-tetraol(15),gymconopin C(16),(2,3-trans)-2-(4-hydroxy-3-methoxyphenyl)-3-hydroxymethyl-10-methoxy-2,3,4,5-tetrahydro-phenanthro[2,1-b]furan-7-ol(17),shanciol(18)...
April 2017: Zhongguo Zhong Yao za Zhi, Zhongguo Zhongyao Zazhi, China Journal of Chinese Materia Medica
Vandana B Patel, Aishwarya D Patel, Dimal A Shah
BACKGROUND: Aspirin combination is prescribed for the its thrombolytic activity where gastric ulceration is the major side effects of aspirin which can be prevented by combining it with proton pump inhibitor omeprazole. Present study describes development of analytical method for the estimation of aspirin and omeprazole in combination. Objective of the present study was to develop and validate chromatographic method for simultaneous analysis of aspirin and omeprazole. METHODS: Isocratic, reversed phase stability indicating liquid chromatographic method was developed for the simultaneous determination of Aspirin and Omeprazole in combination...
October 23, 2017: Current Drug Discovery Technologies
G Naldini, B Fabiani, C Menconi, I Giani, G Toniolo, D Mascagni, J Martellucci
BACKGROUND: In recent years, stapled transanal resection (STARR) has been adopted worldwide with convincing short-term results. However, due to the high recurrence rate and some major complications after STARR, there is still controversy about when the procedure is indicated. The aim of this study was to assess the safety, efficacy and feasibility of STARR performed with a new dedicated device for tailored transanal stapled surgery. METHODS: All the consecutive patients affected by obstructed defecation syndrome (ODS) due to rectocele or/and rectal intussusception, who underwent STARR with the TST STARR-Plus stapler, were included in a prospective study...
October 23, 2017: Techniques in Coloproctology
Linlin Deng, Qianna Zhen, Jieying Gao, Mingchao Jin, Min Ding, Biao Xu
A high performance liquid chromatographic (HPLC) method with fluorescence detection (FD) was established to simultaneously determine plasma indole and skatole. Plasma samples were pretreated by liquid-liquid extraction. Chromatographic separation was accomplished on a Shim-Pack VP-ODS column (150 mm×4. 6 mm, 4.6 μ m) using an isocratic mixture of 15 mmol/L sodium dihydrogen phosphate solution and methanol (40:60, v/v). The fluorescence excitation and emission wavelengths were 274 nm and 340 nm, respectively...
July 8, 2017: Se Pu, Chinese Journal of Chromatography
Xinjie Wang, Jiyu Wang, Heng Li, Xian Hui, Wenyun Gao
A method was developed for the determination of diacetyl in liquors by high performance liquid chromatography-ultraviolet (HPLC-UV) coupled with precolumn derivatization using derivatization reagent 3,3'-diaminobenzidine (DAB). Diacetyl reacted with DAB at room temperature for 10 min. Then the separation was carried out on a high performance liquid chromatograph equipped with a diode array detector (DAD). A Shim-pack VP-ODS (250 mm×4.6 mm, 4.6 μ m) column was employed using water-methanol mobile phases for gradient at a flow rate of 0...
August 8, 2017: Se Pu, Chinese Journal of Chromatography
Yan Li, Longxing Wang, Xiuhua Zhu, Yuan Gao, Jiping Chen
A high performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) method was developed for the determination of hexabromocyclododecanes (HBCDs) in ambient air samples. The samples were extracted by Soxhlet extractor with hexane, then purified on the composite gel column. At first, the interfering substances were rinsed with 50 mL hexane and 100 mL hexane-dichloromethane (9:1, v/v), then 180 mL hexane -dichloromethane (4:1, v/v) was used to elute the targets. The compounds were separated by gradient elution with acetonitrile-methanol-water as mobile phases on a UF-ODS column (150 mm×2...
October 8, 2017: Se Pu, Chinese Journal of Chromatography
Surya N Meena, Mahesh S Majik, Sanjeev C Ghadi, Santosh G Tilve
Grewia nervosa is herbal plant used as traditional medicine for different purposes. Bioassay-guided chemical fractionation of G. nervosa roots resulted in an identification of two known and one new compound, named Microgrewiapine A, Homomicrogrewiapine and N-methyl-microcosamine respectively. Their structures were determined using combination of LC-HRMS, (1) H NMR and IR spectra analyses followed by comparison with those reported in the literature. The problematic separation of these alkaloids on traditional column chromatography (Silica gel, Octadecyl silane (ODS), Sephadex) was resolved by using HPLC method...
October 16, 2017: Chemistry & Biodiversity
Liang Shang, Chuanjun Liu, Yoichi Tomiura, Kenshi Hayashi
Gas chromatography/olfactometry (GC/O) has been used in various fields as a valuable method to identify odor-active components from a complex mixture. Since human assessors are employed as detectors to obtain the olfactory perception of separated odorants, the GC/O technique is limited by its subjectivity, variability, and high cost of the trained panelists. Here, we present a proof-of-concept model by which odor information can be obtained by machine-learning-based prediction from molecular parameters (MPs) of odorant molecules...
November 7, 2017: Analytical Chemistry
Yin-Jun Yang, Xin-Guang Sun, Jie Yang, Qi Li, Jie Zhang, Yang Zhao, Bai-Ping Ma, Bao-Lin Guo
To compare the differences of main components between in rhizoma and fibrous root of Trillium tschonoskii and T. kamtschaticum, a simple, accurate and reliable high performance liquid chromatography coupled with the charged aerosol detector (HPLC-CAD) method was developed and then successfully applied for simultaneous quantitative analysis of three compounds, including polyphyllin Ⅶ (T1),pennogenin 3-O-α-L-rhamnopyranosyl-(1→2) [α-L-rhamnopyranosyl-(1→4)]-β-D-glucopyranoside (T2),polyphyllin Ⅵ (T3), in 16 batches of rhizome and 14 batches of fibrous root...
March 2017: Zhongguo Zhong Yao za Zhi, Zhongguo Zhongyao Zazhi, China Journal of Chinese Materia Medica
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