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Biomedical Chromatography: BMC

Guangyan Du, Lingling Fu, Jun Jia, Xu Pang, Haiyang Yu, Youcai Zhang, Guanwei Fan, Xiumei Gao, Lifeng Han
A rapid, sensitive and specific ultra high performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) method was developed to investigate the pharmacokinetics and tissue distribution of Eclipta prostrata extract. Rats were orally administrated the 70% ethanol extract of E. prostrata, and their plasma as well as various organs were collected. The concentrations of seven main compounds, including ecliptasaponin IV, ecliptasaponin A, apigenin, 3'-hydroxybiochanin A, luteolin, luteolin-7-O-glucoside, and wedelolactone, were quantified by UPLC-MS/MS through multiple reactions monitoring (MRM) method...
January 19, 2018: Biomedical Chromatography: BMC
Ping Guo, Jingjing Zhang, Xiaohui Chen, Longshan Zhao
A molecularly imprinted polymer was synthesized and applied as a sorbent in the solid-phase extraction device. The imprinted polymer was characterized by fourier-transform infrared spectroscopy and scanning electron microscope. The results revealed that imprinted polymer possess sensitive selectivity and reliable adsorption properties for five NSAIDs. The imprinted polymer was successfully applied to the pre-concentration for five NSAIDs in different water samples prior to UPLC-MS/MS. In the early studies, several factors were investigated, including pH adjustment, the kind of elution solvent and the volume of elution solvent...
January 19, 2018: Biomedical Chromatography: BMC
Dan Li, Gang Zhao, Weipeng Ai, Gao Li, Luqin Si, Jiangeng Huang, Yunzhou Chen, Sanlan Wu
In this study, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated to simultaneously determine the anticancer drugs etoposide and paclitaxel in mouse plasma and tissues including liver, kidney, lung, heart, spleen and brain. The analytes were extracted from the matrices of interest by liquid-liquid extraction using DCM: MTBE (1:1, v/v). Chromatographic separation was achieved on an Ultimate XB-C18 column (100 mm × 2.1 mm, 3 μm) at 40 °C and the total run time was 4 min under a gradient elution...
January 19, 2018: Biomedical Chromatography: BMC
Denise Schimek, Reingard Raml, Kevin A Francesconi, Manfred Bodenlenz, Frank Sinner
Time-concentration curves for the topical anti-viral drug acyclovir can provide valuable information for drug development. Open flow microperfusion (OFM) is used for continuous sampling of dermal interstitial fluid but it requires validated methods for subsequent sample analysis. Therefore, we developed a sensitive, selective and high throughput ultra-high-performance liquid chromatography-high resolution tandem mass spectrometry (UHPLC-HR MS/MS) method to determine acyclovir in human dermal interstitial fluid and serum...
January 19, 2018: Biomedical Chromatography: BMC
Nannan Wang, Xiaoning Zhao, Yiran Li, Congcong Cheng, Jiaxin Huai, Kaishun Bi, Ronghua Dai
To reveal the material basis of Huo Luo Xiao Ling Dan, a sensitive and selective ultra-high performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry (UHPLC-Q-TOF/MS) method was developed to identify the absorbed components and metabolites in rat plasma after oral administration of HLXLD. The plasma samples were pretreated by liquid-liquid extraction and separated on a Shim-pack XR-ODS C18 column (75 mm × 3.0 mm, 2.2 μm) using a gradient elution program. With the optimized conditions and single sample injection of each positive or negative ion mode, a total of 109 compounds, including 78 prototype compounds and 31 metabolites were identified or tentatively characterized...
January 19, 2018: Biomedical Chromatography: BMC
Jinfeng Fu, Songyan Wu, Min Wang, Yuan Tian, Zunjian Zhang, Rui Song
Rhizoma et Radix Polygoni Cuspidati (RRPC) is commonly prescribed for the treatments of amenorrhea, arthralgia, jaundice and abscess in traditional Chinese medicine. Previous pharmacological studies have indicated that polyphenols are the main pharmacological active ingredients in RRPC. Meanwhile, the poor bioavailability of polyphenols in RRPC implies that those components are probably metabolized by intestinal bacteria before absorption. However, there is rather limited information about RRPC's metabolites produced by intestinal bacteria and the intestinal absorbed constituents...
January 15, 2018: Biomedical Chromatography: BMC
Min-Ji Kim, Seung-Hwan Kwon, Choon-Gon Jang, Han-Joo Maeng
A simple, sensitive and rapid liquid chromatography tandem mass spectrometry method (LC-MS/MS) was developed and validated for the determination of plasma isoorientin levels in rats. After simple protein precipitation using methanol, chromatographic analysis was performed using a Synergi 4μ polar-RP 80A column (150 mm × 2.0 mm, 4 μm) under isocratic conditions and a mobile phase consisting of 0.1% formic acid in water and methanol (80:20, v/v) at a flow rate of 0.2 mL/min. In positive electrospray ionization mode, the protonated precursor and product ion transitions of isoorientin (m/z 449...
January 15, 2018: Biomedical Chromatography: BMC
Yun-Qing Li, Cheng-Jian Li, Lei Lv, Qing-Qing Cao, Xian Qian, Si Wei Li, Hui Wang, Liang Zhao
Stellerachamaejasme L. has been used as a Traditional Chinese Medicine for the treatment of scabies, tinea, stubborn skin ulcers, chronic tracheitis, cancer and tuberculosis. A sensitive and selective ultra-high liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the simultaneous determination of five flavonoids (stelleranol, chamaechromone, neochamaejasmin A, chamaejasmine and isochamaejasmin) of Stellerachamaejasme L. in rat plasma. Chromatographic separation was accomplished on an Agilent Poroshell 120 EC-C18 column (2...
January 12, 2018: Biomedical Chromatography: BMC
Narayan Balaji, Suresh P Sulochana, Neeraj Kumar Saini, A Siva Kumar, Ramesh Mullangi
A simple, selective and reliable LC-MS/MS method was validated for simultaneous quantitation of darolutamide diastereomers in 50 μL mice plasma using warfarin as an internal standard (IS) as per regulatory guidelines. Plasma samples were extracted by liquid-liquid extraction and the chromatographic separation was achieved on a Chiralpak IA column with an isocratic mobile phase 5 mM ammonium acetate:absolute alcohol (20:80, v/v) at a flow rate of 1.0 mL/min. Detection and quantitation was done by MRM mode following the transitions: m/z 397 → 202 and 307 → 250 for darolutamide diastereomers and the IS, respectively in the negative ionization mode...
January 8, 2018: Biomedical Chromatography: BMC
Wenjing Zhang, Sihui Wan, Lizhi Chen, Xuebing Wang, Zhuo Wang, Yi Huang
A new method for the analysis of cycloserine (4-amino-3-isoxazolidinone, CYC) in rat microdialysis samples has been developed. This method consists of derivatizing the CYC with benzoyl chloride, which transforms primary amines into highly stable derivatives. An attractive feature of this method was that the derivatization reaction is straightforward and can be completed within 10 min. The formed derivative, in contrast to the non-derivatized analyte, exhibited increased chromatographic retention and decreased matrix effects resulting from the co-elution of other components using reversed-phase liquid chromatography and on-line switching...
January 4, 2018: Biomedical Chromatography: BMC
Xiaopeng Chen, Kyla M Walter, Galen W Miller, Pamela J Lein, Birgit Puschner
Environmental toxicants that interfere with thyroid hormone (TH) signaling can impact growth and development in animals and humans. Zebrafish represent a model to study chemically-induced TH disruption, prompting the need for sensitive detection of THs. Simultaneous quantification of 3,3',5-triiodo-L-thyronine (T3), thyroxine (T4), 3,3',5'-triiodo-L-thyronine (rT3), 3,5-diiodo-L-thyronine (3,5-T2), and 3,3'-diiodo-L-thyronine (3,3'-T2) in zebrafish larvae was achieved by ultra-performance liquid chromatography-tandem mass spectrometry in positive ion mode...
January 3, 2018: Biomedical Chromatography: BMC
Jutta Lintelmann, Xiao Wu, Evelyn Kuhn, Sebastian Ritter, Claudia Schmidt, Ralf Zimmermann
A high performance liquid chromatographic (HPLC) method with integrated solid phase extraction (SPE) for the determination of 1-hydroxypyrene and 1-; 2-; 3-; 4- and 9-hydroxyphenanthrene in urine was developed and validated. After enzymatic treatment and centrifugation of 500 μl urine, 100 μl of the sample were directly injected into the HPLC-system. Integrated SPE was performed on a selective, copper phthalocyanine modified packing material. Subsequent chromatographic separation was achieved on a pentafluorophenyl (PFP) core-shell column by using a methanol gradient...
January 3, 2018: Biomedical Chromatography: BMC
Ola M Abdallah, Ahmed M Abdel-Megied, Amira S Gouda
The first simple and highly sensitive Liquid chromatography-tandem mass spectrometry (LC-MS/MS) bioanalytical method was developed and fully validated for the simultaneous determination of newly discovered antiviral drugs namely, Sofosbuvir (SOF) and Daclatasvir (DAC) in human plasma. Tadalafil (TAD) was used as internal standard (IS). SOF, DAC and TAD (IS) were extracted from plasma using liquid-liquid extraction technique with methyl tert-butyl ether. The chromatographic separation was carried out using ZorbaxSB-C18 column (4...
January 3, 2018: Biomedical Chromatography: BMC
Jin-Qi Li, Jia-Feng Wang, Jie Li, Shu-Han Zhang, Dan He, Rong-Sheng Tong, Shu-Ya She
Senkyunolide I is one of the major bioactive components in herb medicine Ligusticum chuanxiong. The aim of this study was to develop and validate a fast, simple and sensitive LC-MS/MS method for the determination of senkyunolide I in dog plasma. The plasma samples were processed with acetonitrile and separated on a Waters ACQUITY UPLC BEH C18 column (50 × 2.1 mm, 1.7 μm). A mobile phase consisted of 0.1% formic acid aqueous and acetonitrile was delivered at a flow rate of 0.3 mL·min-1 . The detection was achieved in the positive selected reaction monitoring (SRM) mode with precursor-to-product transitions at m/z 225...
January 3, 2018: Biomedical Chromatography: BMC
Shinya Takasaki, Masaki Tanaka, Masafumi Kikuchi, Masamitsu Maekawa, Yoshihide Kawasaki, Akihiro Ito, Yoichi Arai, Hiroaki Yamaguchi, Nariyasu Mano
An analytical method using high performance liquid chromatography/electrospray ionization tandem mass spectrometry has been developed and validated for simultaneous measurement of four tyrosine kinase inhibitors used for renal cell carcinoma and their metabolites in human plasma. Despite their similar structures, it is difficult to measure plasma levels of these compounds simultaneously using optimal MS parameters for each compound because a quantitative range exceeding 50,000-fold is required. To overcome this problem, we used a linear range shift technique using in-source collision-induced dissociation...
December 28, 2017: Biomedical Chromatography: BMC
Xiaotao Zhang, Hongwei Hou, Huan Chen, Yong Liu, An Wang, Qingyuan Hu
The discovery of new laryngeal cancer-related metabolite biomarkers could help to facilitate early diagnosis. A serum metabolomics study from laryngeal cancer patients and healthy individuals was conducted by using liquid chromatography coupled with quadrupole time-of-flight mass spectrometry. Univariate and multivariate statistics were used to discriminate laryngeal cancer patients and healthy individuals. 1-palmitoyl-sn-glycero-3-phosphocholine (LysoPC 16:0), 1-o-hexadecyl-2-acetyl-sn-glycero-3-phosphocholine (PAF), 1,2-dipalmitoyl-sn-glycero-3-phosphocholine were found to be significantly different between laryngeal cancer group and healthy group...
December 22, 2017: Biomedical Chromatography: BMC
Bogdan I Cioroiu, Ioana C Caba, Irina Prisăcaru, Mona E Cioroiu, Mihai I Lazar, Marius Niculaua
Fenspiride hydrochloride (FNS) is used in treating chronic inflammatory diseases, most commonly as a liquid oral solution. FNS produces degradation products along with fenspiride N-oxide (FNO) and 1-phenylethyl-4-hydroxy-4-aminomethyl piperidine hydrochloride (PHAP). We aimed to develop and validate a chromatographic method in order to identify the main degradation products in the presence of other compounds from a liquid preparation. The method used a dual gradient using two buffer solutions; first with pH 4...
December 19, 2017: Biomedical Chromatography: BMC
Kazuhiro Tanabe, Koji Matsuo, Masaki Miyazawa, Masaru Hayashi, Masae Ikeda, Masako Shida, Takeshi Hirasawa, Ryuichiro Sho, Mikio Mikami
Serum levels of fully sialylated C4-binding protein (FS-C4BP) are remarkably elevated in patients with epithelial ovarian cancer (EOC) and can be used as a marker to distinguish ovarian clear cell carcinoma from endometrioma. This study aimed to develop a stable, robust, and reliable liquid chromatography- hybrid mass spectrometry (UPLC-MS/MS) based diagnostic method that would generalize FS-C4BP as a clinical EOC biomarker. Glycopeptides derived from 20 μL of trypsin-digested serum glycoprotein were analyzed via UPLC equipped with electrospray ionization time-of-flight mass spectrometer...
December 18, 2017: Biomedical Chromatography: BMC
Junguo Liu, Jiuxue Song, Karen Huang, Deborah Michel, Jim Fang
A high performance liquid chromatography tandem-mass spectrometry (HPLC-MS/MS) method has been developed to analyze anthocyanins in urine and plasma to further understand their absorption, distribution, metabolism and excretion. The method employed a Synergi RP-Max column (250 x 4.6 mm, 4 μm) and an API 4000 mass spectrometer. A gradient elution system consisted of mobile phase A (water/1% formic acid) and mobile phase B (acetonitrile) with a flow rate of 0.60 ml/min. The gradient was initiated at 5% B, increased to 40% B at 15 min, and then increased to 100% B at 22 min...
December 18, 2017: Biomedical Chromatography: BMC
Xia Gao, Yuling Ma, Zhuowei Wang, Ruibin Bia, Pei Zhang, Fangdi Hu
The dried roots of Inula helenium L. (IH) and Inula racemosa Hook f. (IR) are used commonly as folk medicine as "tumuxiang" (TMX). The mixing and sharing of IH and IR in clinical use is a universal phenomenon. Modern pharmacological studies confirmed that IH and IR display anti-inflammatory activities. However, the difference in anti-inflammatory pharmacodynamic substances between these two herbs is still unknown. In the present study, the fingerprints of 18 IH and 9 IR samples were established by using UPLC/QTOF-MSE ...
December 18, 2017: Biomedical Chromatography: BMC
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