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Adnan A Kadi, Hany W Darwish, Mohamed W Attwa, Sawsan M Amer
In the current work, a rapid, specific, sensitive and validated liquid chromatography tandem mass-spectrometric method was developed for the quantification of ponatinib (PNT) in human plasma and rat liver microsomes (RLMs) with its application to metabolic stability. Chromatographic separation of PNT and vandetanib (IS) were accomplished on Agilent eclipse plus C18 analytical column (50 mm × 2.1 mm, 1.8 μm particle size) maintained at 21±2°C. Flow rate was 0.25 mLmin-1 with run time of 4 min. Mobile phase consisted of solvent A (10 mM ammonium formate, pH adjusted to 4...
2016: PloS One
T Jayasena, A Poljak, N Braidy, L Zhong, B Rowlands, J Muenchhoff, R Grant, G Smythe, C Teo, M Raftery, P Sachdev
Sirtuin proteins have a variety of intracellular targets, thereby regulating multiple biological pathways including neurodegeneration. However, relatively little is currently known about the role or expression of the 7 mammalian sirtuins in the central nervous system. Western blotting, PCR and ELISA are the main techniques currently used to measure sirtuin levels. To achieve sufficient sensitivity and selectivity in a multiplex-format, a targeted mass spectrometric assay was developed and validated for the quantification of all seven mammalian sirtuins (SIRT1-7)...
October 20, 2016: Scientific Reports
Bin Liu, Jiaojiao Lu, Chunqing Ai, Bao Zhang, Li Guo, Shuang Song, Beiwei Zhu
Uronic acid-containing polysaccharides (UACPs) including well-known glycosaminoglycans (GAGs) and some non-GAGs exist widely in animal kingdom. Although numerous methods have been established to analyze GAGs, few methods are available for non-GAG UACPs. In the present study, a protocol to identify all kinds of UACPs with repeating disaccharide units of hexosamine and uronic acid was demonstrated, and UACP components in five shellfishes, namely Turritella fortilirata Sowerby (GTF), Batillaria zonalis (GBZ), Nassarius variciferus (GNV), Monodonta labio Linnaeus (GML), and Argopecten irradians Lamarck (BAI) were primarily revealed...
October 11, 2016: Carbohydrate Research
Artem D Rogachev, Olga I Yarovaya, Sergey V Ankov, Mikhail V Khvostov, Tatyana G Tolstikova, Andrey G Pokrovsky, Nariman F Salakhutdinov
A fast, selective and sensitive procedure for quantitation of the camphor-based anti-influenza agent camphecene in whole rat blood was developed and validated using dried blood spots and LC-MS/MS. The method was validated according to recommendations of the FDA and EMA in terms of selectivity, linearity, accuracy, precision, recovery, matrix factor, stability, and carry-over. Sample preparation included spotting 20μL of whole blood taken from the tail vein onto the paper, drying and extracting the analyte, followed by evaporation of the solvent and analysis of the residue...
October 11, 2016: Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences
Chuan-Han Chen, Jeon-Hor Chen, Hung-Chieh Chen, Jyh-Wen Chai, Po-Lin Chen, Clayton Chi-Cheng Chen
BACKGROUND: Diagnosis of spontaneous intracranial hypotension (SIH) relies on the ability of medical staff to recognize cerebrospinal fluid (CSF) leakage at the spine. However, difficulties with interobserver discrepancy sometimes occurred while reading magnetic resonance myelography (MRM) because clear image definition was lacking. In this study, we tried to determine which pattern of CSF distribution is more reliable for diagnosis of CSF leakage by using MRM. METHODS: From January 2012 to August 2014, 19 SIH patients and 27 healthy controls (HC) were recruited into our study; 10 of the 19 patients were recovered (SIH-R) after treatment...
October 12, 2016: Journal of the Chinese Medical Association: JCMA
Shiyue Zhou, Kerry M Wooding, Yehia Mechref
The development of a reliable and high-throughput glycomic profiling strategy is in high demand due to the biological roles of glycans and their association with different diseases. Native analysis can be quite difficult because of the low ionization efficiency and microheterogeneity of glycans. In this chapter, the sample preparation protocols and LC-MS analysis of permethylated glycan strategies are introduced. Solid-phase permethylation is a fast, convenient, and high-yield method to stabilize sialic acid and improve glycan ionization efficiency and analysis in positive mode; this results in a more sensitive and reliable glycomic profiling strategy...
2017: Methods in Molecular Biology
Ravali Alagandula, Xiang Zhou, Baochuan Guo
RATIONALE: LC-MS/MS is the gold standard of urine drug testing. However, current LC-based methods are time consuming, limiting the throughput of MS-based testing and increasing the cost. This is particularly problematic for quantification of drugs such as phenobarbital, which is often analyzed in a separate run because they must be negatively ionized. METHOD: This study examined the feasibility of using a dilute and shoot-flow injection method without LC separation to quantify drugs with phenobarbital as a model system...
October 14, 2016: Rapid Communications in Mass Spectrometry: RCM
Yongrui He, Xian-En Zhao, Renjun Wang, Na Wei, Jing Sun, Jun Dang, Guang Chen, Zhiqiang Liu, Shuyun Zhu, Jin-Mao You
A simple, rapid, sensitive, selective and environmentally friendly method, based on in situ derivatization ultrasound-assisted dispersive liquid-liquid microextraction (in situ DUADLLME) coupled with ultra high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) using multiple reaction monitoring (MRM) mode has been developed for the simultaneous determination of food-related biogenic amines and amino acids. A new mass spectrometry sensitive derivatization reagent 4'-carbonyl chloride rosamine (CCR) was designed, synthesized and firstly reported...
October 14, 2016: Journal of Agricultural and Food Chemistry
Qiang Ren, Lin Ding, Shan-Shan Sun, Hui-Yun Wang, Liang Qu
Lycopus lucidus Turcz has been used as a traditional phytomedicine for menstrual disorder, amenorrhea, menstrual cramps, inflammation, and cardiovascular diseases. However, there is not enough information about identification and quantification for the chemical constituents of L. lucidus Turcz. In this work, a simple, rapid, and sensitive UHPLC - Q-TOF-MS method was developed for characterization and identification of the phytochemical compositions in L. lucidus Turcz in negative ion mode. A total of 37 compounds, including 15 phenolic acids, 12 flavonoids, 3 triterpenoids, and 7 organic acids were tentatively characterized and identified by means of the retention time, accurate mass and characteristic fragment ions...
October 14, 2016: Biomedical Chromatography: BMC
Yachun Su, Liping Xu, Zhuqing Wang, Qiong Peng, Yuting Yang, Yun Chen, Youxiong Que
BACKGROUND: Sugarcane smut, which is caused by Sporisorium scitamineum, has been threatening global sugarcane production. Breeding smut resistant sugarcane varieties has been proven to be the most effective method of controlling this particular disease. However, a lack of genome information of sugarcane has hindered the development of genome-assisted resistance breeding programs. Furthermore, the molecular basis of sugarcane response to S. scitamineum infection at the proteome level was incomplete and combining proteomic and transcriptional analysis has not yet been conducted...
October 12, 2016: BMC Genomics
Juntuo Zhou, Yuxin Yin
Advances in liquid chromatography-mass spectrometry (LC-MS) instruments and analytical strategies have brought about great progress in targeted metabolomics analysis. This methodology is now capable of performing precise targeted measurement of dozens or hundreds of metabolites in complex biological samples. Classic targeted quantification assay using the multiple reaction monitoring (MRM) mode has been the foundation of high-quality metabolite quantitation. However, utilization of this strategy in biological studies has been limited by its relatively low metabolite coverage and throughput capacity...
October 10, 2016: Analyst
Chang-Cai Liu, Gui-Lan Huang, Hai-Ling Xi, Shi-Lei Liu, Jing-Quan Liu, Hui-Lan Yu, Shi-Kun Zhou, Long-Hui Liang, Ling Yuan
This work describes a novel and sensitive non-isotope dilution method for simultaneous quantification of organophosphorus nerve agents (OPNAs) soman (GD) and VX adducts to butyrylcholinesterase (BChE), their aged methylphosphonic acid (MeP) adduct and unadducted BChE in plasma exposed to OPNA. OPNA-BChE adducts were isolated with an off-column procainamide-gel separation (PGS) from plasma, and then digested with pepsin into specific adducted FGES(*)AGAAS nonapeptide (NP) biomarkers. The resulting NPs were detected by UHPLC-MS/MS MRM...
October 3, 2016: Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences
Yi Tao, Yuchao Ren, Weidong Li, Baochang Cai, Liuqing Di, Liyun Shi, Lihong Hu
The purpose of this study is to establish and validate an UPLC-MS/MS approach to determine 4-caffeoylquinic acid, chlorogenic acid, 3,5-dicaffeoylquinic acid, loganic acid, loganin, sweroside, dipsacoside B and asperosaponin VI from extracts of crude and wine-processed Dipsacus asper in biological samples and apply the approach to a comparative pharmacokinetic study. A Waters BEH C18 UPLC column was employed with acetonitrile/0.2% formic acid-water as mobile phases. The mass analysis was carried out in a triple quadrupole mass spectrometer using multiple reaction monitoring (MRM) with negative scan mode...
September 30, 2016: Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences
Anne H Calhoun, Nicole Gill
BACKGROUND: This retrospective observational study describes what appears to be a not-uncommon yet not previously typified headache disorder, "end-menstrual migraine" (EMM) named for its proximate occurrence with the terminal days of menstrual bleeding each month. METHODS: Our menstrual migraine (MM) clinic's database was queried for patients with migraine, regular menses, and the locally used diagnostic code of EMM, signifying the patient's assertion that she had migraine at the end of menses as well as calendar data confirming that association...
October 5, 2016: Headache
Hwang Eui Cho, H Kang Min
A simple and accurate high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of N-(4-hydroxyphenyl)retinamide (fenretinide, 4-HPR) and its metabolites, 4-oxo-N-(4-hydroxyphenyl)retinamide (4-oxo-4-HPR) and N-(4-methoxyphenyl)retinamide (4-MPR), in human plasma. Plasma samples were prepared using protein precipitation with ethanol. Chromatographic separation of the three analytes and N-(4-ethoxyphenyl)retinamide (4-EPR), an internal standard, was achieved on a Zorbax SB-C18 column (3...
September 29, 2016: Journal of Pharmaceutical and Biomedical Analysis
Shuna Jin, Chengwu Song, Shuailong Jia, Sen Li, Yang Zhang, Cheng Chen, Yulin Feng, Yong Xu, Chaomei Xiong, Yi Xiang, Hongliang Jiang
Turmeric and curcuminoids are used as natural food coloring and functional food additives in various parts of the world. In this study, ninety-six curcuminoids were fully characterized using a targeted curcuminoid profile, which established by integrated use of two complementary LC-MS/MS platforms (liquid chromatography-quadrupole time of flight mass spectrometry (LC-QTOF-MS/MS) and liquid chromatography-quadrupole linear ion trap mass spectrometry (LC-QTRAP-MS/MS)). The curcuminoid profile was represented in the form of a multiple reaction monitoring (MRM) mode based on LC-QTRAP-MS/MS analysis...
September 27, 2016: Journal of Pharmaceutical and Biomedical Analysis
Roberto Stella, Federica Barrucci, Roberto Angeletti, Peter James, Clara Montesissa, Giancarlo Biancotto
The illegal use of pharmacologically active compounds for growth promotion in food-producing species poses risks for consumer health and animal welfare. Surveillance relies on the quantification of drug residues in animal fluids or tissues, but the efficacy can be negatively affected due to undetectable residual concentrations in biological matrices. Consequently, techniques focusing on the indirect biological effects of exogenous compound administration have been proposed as more sensitive detection methods...
September 30, 2016: Analytical and Bioanalytical Chemistry
Man-Yun Chen, Yong-Jun Tang, Yi-Cheng Wang, Chong-Zhi Wang, Chun-Su Yuan, Yao Chen, Zhi-Rong Tan, Wei-Hua Huang, Hong-Hao Zhou
The compound medicine of betamethasone sodium phosphate (BSP) and betamethasone dipropionate (BDP) is widely used for diverse glucocorticoid-sensitive acute and chronic diseases such as asthma, rheumatoid arthritis and systemic lupus erythematosus. It will be useful and beneficial to validate sensitive method for the determination of BSP, BDP and their metabolites for their pharmacokinetic study. Hereby, an ultra-high pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been validated for the determination of BSP, BDP and their metabolites betamethasone (BOH), betamethasone 17-monodipropionate (B17P) and betamethasone 21-monodipropionate (B21P) in human plasma...
May 7, 2016: Analytical Methods: Advancing Methods and Applications
Miloslav Sanda, Julius Benicky, Jing Wu, Yiwen Wang, Kepher Makambi, Jaeil Ahn, Coleman I Smith, Peng Zhao, Lihua Zhang, Radoslav Goldman
BACKGROUND: Non-invasive monitoring of liver disease remains an important health issue. Liver secreted glycoproteins reflect pathophysiological states of the organ and represent a rational target for serologic monitoring. In this study, we describe sialylated O-glycoforms of liver-secreted hemopexin (HPX) and quantify them as a ratio of disialylated to monosialylated form (S-HPX). METHODS: We measured S-HPX in serum of participants of the HALT-C trial using a LC-MS/MS-MRM assay...
2016: Clinical Proteomics
Andrew J Percy, Sarah A Michaud, Armando Jardim, Nicholas J Sinclair, Suping Zhang, Yassene Mohammed, Andrea L Palmer, Darryl B Hardie, Juncong Yang, Andre M LeBlanc, Christoph H Borchers
The mouse is the most commonly used laboratory animal, with more than 14 million mice being used for research each year in North America alone. The number and diversity of mouse models is increasing rapidly through genetic engineering strategies, but detailed characterization of these models is still challenging because most phenotypic information is derived from time-consuming histological and biochemical analyses. To expand the biochemists' toolkit, we generated a set of targeted proteomic assays for mouse plasma and heart tissue, utilizing bottom-up LC/MRM-MS with isotope-labeled peptides as internal standards...
September 30, 2016: Proteomics
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