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Biomedical Chromatography: BMC

Fulin Jiang, Xiang Peng, Dake Cai, Dingsheng Wen, Yao Liu, Min Zhi, Jiangying Chen, Pinjin Hu, Xueding Wang, Yujie Gao, Min Huang, Xiang Gao, Guoping Zhong
An accurate and sensitive LC-MS/MS method for determining thalidomide, 5-hydroxy thalidomide and 5'-hydroxy thalidomide in human plasma was developed and validated using umbelliferone as an internal standard. The analytes were extracted from plasma (100 μL) by liquid-liquid extraction with ethyl acetate and then separated on a BETASIL C18 column (4.6 mm×150 mm, 5μm) with mobile phase composed of methanol / water containing 0.1% formic acid (70/30, v/v) in an isocratic mode at a flow rate of 0.5 ml/min. The detection was performed using an API triple quadrupole mass spectrometer in APCI mode...
March 12, 2018: Biomedical Chromatography: BMC
Ting Tan, Jing Zhang, Xu Xu, Wen-Ping Huang, Yun Luo
Glechomae Herba (GH) is rich in bioactive phenolic constituents, which is widely used for treatment of cholelithiasis, urolithiasis and dropsy. The simultaneous determination of phenolic constituents in GH from different geographical origins is significant for authentication and quality control purposes. In this study, we developed a strategy integrating targeted analysis and chemometric methods for quality evaluation and discrimination of GH from different geographical origins. Firstly, an accurate and reliable liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for simultaneous quantification of fifteen phenolic constituents in GH from different geographical origins...
March 10, 2018: Biomedical Chromatography: BMC
Amer Jamalpoor, Rolf W Sparidans, Carla Pou Casellas, Johannes J M Rood, Mansi Joshi, Rosalinde Masereeuw, Manoe J Janssen
Nephropathic cystinosis is characterized by abnormal intralysosomal accumulation of cystine throughout the body causing irreversible damage to various organs, particularly the kidneys. Cysteamine, the currently available treatment, can reduce lysosomal cystine and postpone disease progression. However, cysteamine poses serious side effects and does not address all symptoms of cystinosis. To screen for new treatment options, a rapid and reliable high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed to quantify cystine in conditionally immortalized human proximal tubular epithelial cells (ciPTEC)...
March 8, 2018: Biomedical Chromatography: BMC
Yanqing Liu, Hongwu Wang, Su Yao, Peijie Zhu
A fast and sensitive method involving ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was introduced to detect citrinin in dried orange peel. A series of extraction, purification, and chromatographic conditions was also systematically examined. With the proposed method, the obtained calibration graph was linear, with an R of 0.9996 within a concentration range of 0.5-10 ng/mL. The estimated limits of detection and quantification were 0.05 and 0.17 ng/mL, respectively. Under the selected conditions, the relative recoveries in different citrus products spiked with 1-10 ng/mL citrinin were 89...
March 8, 2018: Biomedical Chromatography: BMC
Rohini Sidhu, Christina R Mikulka, Hideji Fujiwara, Mark S Sands, Jean E Schaffer, Daniel S Ory, Xuntian Jiang
Deficiencies of galactosylceramidase and glucocerebrosidase result in the accumulation of galactosylsphingosine (GalSph) and glucosylsphingosine (GluSph) in Krabbe and Gaucher diseases, respectively. GalSph and GluSph are useful biomarkers for both diagnosis and monitoring of treatment effects. We have developed and validated a sensitive, accurate, high throughput assay for simultaneous determination of the concentration of GalSph and GluSph in mouse serum. GalSph and GluSph and their deuterated internal standards were extracted by protein precipitation in quantitative recoveries, baseline separated by hydrophilic interaction chromatography, and detected by positive-ion electrospray mass spectrometry in multiple reaction monitoring mode...
March 8, 2018: Biomedical Chromatography: BMC
Lixiang Aa, Fei Fei, Zhaoyi Tan, Jiye Aa, Guangji Wang, Changxiao Liu
Ginkgolides are the primarily active components in Ginkgo products that are popular worldwide. However, few studies have evaluated the bioavailability of ginkgolides and the effects of food on it after oral administration of ginkgolides. In this article, pharmacokinetics and absolute bioavailability of the primary components in ginkgolide extracts were evaluated in beagle dogs. For the first time, we showed that the fed dogs had significantly increased area under the concentration-time curve and peak concentration relative to the fasted dogs based on the data from both the prototype form and total lactones of ginkgolide A (GA) and ginkgolide B (GB)...
March 8, 2018: Biomedical Chromatography: BMC
Lili Li, Jiaxing Chen, Xiaoyan Yang, Yingtao Zhang, Donghui Yang
Isoimperatorin (IP) and phellopterin (PP) are two furocoumarins existed in Angelicae Dahuricae Radix, there is an isopentenyloxyl substituted at C-5 in IP, while an isopentenyloxyl and a methoxyl substituted at C-8 and C-5 in PP, respectively. To elucidate the in vivo metabolic characteristics of PP and IP, HPLC coupled with diode array detector and electrospray ionization ion trap time-of-flight mass spectrometry technique was used. Totally, 110 metabolites, including 53 new ones, were identified from the urine and plasma samples of rats after oral administration of IP and PP, respectively...
March 8, 2018: Biomedical Chromatography: BMC
Yongzhi Tian, Xiao Wu, Mingjie Zhang, Longshan Zhao, Zhili Xiong, Feng Qin
A rapids, selective and sensitive high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed to determine meloxicam in beagle dog plasma. Sample pretreatment involved a one-step protein precipitation with methanol of 0.1 mL plasma. Analysis was performed on a Venusil ASB-C18 column with mobile phase consisting of methanol-water (containing 0.1% formic acid) (75:25, v/v). The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring (MRM) mode via electrospray ionization (ESI) source...
March 5, 2018: Biomedical Chromatography: BMC
Jin-Ju Byeon, Min-Ho Park, Seok-Ho Shin, Byeong Ill Lee, Yuri Park, Jangmi Choi, Nahye Kim, Yeonjae Kang, Young G Shin
A single hybrid affinity-captured-LC-TOF-MS/MS method was developed and applied for the quantification of total antibody, antibody conjugated drug and free payload of antibody drug conjugate (ADC). Adcetris®, one of the valine-citrulline MMAE (vc-MMAE) conjugated ADC, was used as a model ADC compound. A quadratic regression (weighted 1/concentration) was used to fit calibration curves over the concentration range of 30.65-613.00 ng/mL with an equation y=ax2 +bx+c for the acDrug of Adcetris®. The qualification run met the acceptance criteria of ± 25% accuracy and precision values for quality control samples...
March 5, 2018: Biomedical Chromatography: BMC
Dalia Mohamed, Maha A Hegazy, Mona S Elshahed, Safaa S Toubar, Marwa I Helmy
A facile, fast and specific method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the simultaneous quantitation of paracetamol (PAR), chlorzoxazone (CXZ) and aceclofenac (ACL) in human plasma was developed and validated. Sample preparation was achieved by liquid-liquid extraction. The analysis was performed on a reversed-phase C18 HPLC column (5 μm, 4.6× 50 mm) using acetonitrile: 10 mM ammonium formate pH 3.0 (65:35, v/v) as the mobile phase where atrovastatin (ATR) was used as an internal standard...
March 5, 2018: Biomedical Chromatography: BMC
Luyi Zhou, Jing Li, Chong Yan
A selective and sensitive liquid chromatography-tandem mass spectrometry method was developed and validated for investigating the pharmacokinetics of umbelliferone, apigenin, genkwanin, and hydroxygenkwanin after oral administration of Daphne genkwa extract. Plasma samples were treated by protein precipitation with acetonitrile. Analytes were detected by triple-quadrupole MS/MS with an ESI source in negative selection reaction monitoring mode. The transitions of m/z 161→133 for umbelliferone, m/z 269→117 for apigenin, m/z 283→268 for genkwanin, and m/z 299→284 for hydroxygenkwanin were confirmed for quantification...
March 3, 2018: Biomedical Chromatography: BMC
Patrick Neiens, Angela De Simone, Anna Ramershoven, Georg Höfner, Lars Allmendinger, Klaus T Wanner
MS Binding Assays represent a label free alternative to radioligand binding assays. In this study, we present an LC-ESI-MS/MS method for the quantification of (R,R)-4-(2-benzhydryloxyethyl)-1-(4-fluorobenzyl)piperidin-3-ol ((R,R)-D-84, (R,R)-1), (S,S)-reboxetine ((S,S)-2), and (S)-citalopram ((S)-3) employed as highly selective nonlabelled reporter ligands in MS Binding Assays addressing the dopamine (DAT, (R,R)-D-84), the norepinephrine (NET, (S,S)-reboxetine), and the serotonin transporter (SERT, (S)-citalopram), respectively...
March 3, 2018: Biomedical Chromatography: BMC
Haizhen Zhang, Min Huang, Weiwei Yu, A'wei Zhang, Kankan Zhang, Deyu Hu
A simple and rapid method for enantioselective determination of dufulin in cucumber and soil was developed by liquid chromatography with tandem mass spectrometry. The enantiomers were separated on a Superchiral S-OD chiral cellulose tris(3,5-dimethylphenylcarbamate) column at 20 °C, with a mixture of acetonitrile and water (0.1% formic acid) (52:48, v/v) as mobile phase at a flow rate of 0.65 mL/min. The pretreatment conditions were optimized using an orthogonal test, and the optimized method showed good linearity and sensitivity...
March 3, 2018: Biomedical Chromatography: BMC
Caiyuan Sun, Lingrong Zeng, Jin Xu, Lei Zhong, Xinwen Han, Lingzhu Chen, Yuping Zhang, Deyu Hu
In this study, a modified quick, easy, cheap, effective, rugged and safe (QuEChERS) method coupled with gas chromatography (GC) with electron capture detection (ECD) was established to determine dimethachlon residues in paddy soil, rice husk, rice straw, brown rice and cooked rice. The limits of quantification of dimethachlon were 0.01 mg/kg for paddy soil, brown rice and cooked rice and 0.02 mg/kg for rice straw and rice husk. The mean recoveries were in the range 78.59%-104.7% with relative standard deviation R-values of <10% for dimethachlon in the five matrices...
March 3, 2018: Biomedical Chromatography: BMC
Lian-Jie Ren, Hua-Jing Wu, Li-Han Sun, Xue Xu, Li-Ying Mo, Lei Zhang, Jun-Ying Zhang, Chun-Yong Wu
Cabozantinib (CBZ) could be used for the treatment of progressive, metastatic medullary thyroid cancer. Its major oxidative metabolite is cabozantinib N-oxide (CBN) which contains a structural alert associated with mutagenicity, yet the pharmacokinetics study lacks the simultaneous investigation of CBN and dose proportionality. In current study a simple LC-MS/MS method was developed and validated for the simultaneous estimation and pharmacokinetic investigation of CBZ and CBN in rat plasma. The analytes were separated on a Waters Atlantics C18 column (2...
March 3, 2018: Biomedical Chromatography: BMC
Mamdouh R Rezk, Kamal A Badr
A robust, rapid and sensitive UPLC-MS/MS method has been developed, optimized and validated for determination of amlodipine (AML) and atorvastatin (ATO) in human plasma using eplerenone as an internal standard (IS). Multiple-reaction monitoring in positive electrospray ionization mode was utilized in Xevo TQD LC-MS/MS. Double extraction was used in sample preparation using diethyl ether and ethyl acetate. The prepared samples were analyzed using Acquity UPLC BEH C18 (50 x 2.1 mm, 1.7 μm) column. Ammonium formate and acetonitrile, pumped isocraticaly at a flow rate of 0...
March 2, 2018: Biomedical Chromatography: BMC
Banghua Meng, Yurong Yu, Qingtao Zhang, Shouyi Wang, Deyu Hu, Kankan Zhang
A simple analytical method was developed to simultaneously determine thiamethoxam and its metabolite, clothianidin, in fresh tobacco leaf, soil, and cured tobacco leaf using liquid chromatography with tandem mass spectrometry. Thiamethoxam and clothianidin in tobacco and soil samples were extracted with acetonitrile containing 0.1% formic acid and purified using an NH2 -SPE column. The optimized method provided good linearity with coefficients of determination R2 ≥ 0.9981. The limits of detection and quantification were in between 0...
March 2, 2018: Biomedical Chromatography: BMC
Zhixiong Zhong, Gongke Li, Lingchuan Guo, Jing Yao, Zhe Liu, Jianchao Deng
A highly sensitive method was developed for the analysis of short-chain perfluorinated alkyl acids (PFAAs) in serum samples using solid-phase extraction (SPE) coupled with ion chromatography-electrospray ionization-mass spectrometry. The synthesized amino-functionalized graphene oxide nanocomposites were used as a SPE sorbent for the enrichment of trace analytes and purification of samples. It exhibited high selectivity to polar compounds. The suppressor was employed to remove counterions and reduce background signals of mobile phase...
March 1, 2018: Biomedical Chromatography: BMC
Fernanda Caroline Wolff, Thaís Luise Dillenburg, Marina Venzon Antunes, Rafael Linden, Sandrine Comparsi Wagner, Simone G Verza
Imatinib mesylate (IM) is an anti-neoplasic drug used for the treatment of cancer. Recently new guidelines specify daily doses and concentration limits for genotoxic impurities (GTIs) in pharmaceutical final products. So, in this work an analytical method by UHPLC-MS/MS was developed, validated and applied to characterize IM tablets for two GTIs: N-(2-methyl-5-aminophenyl)-4-(3-pyridyl)-2-pyrimidine amine (Imp. 1), and N-[4-methyl-3-(4-methyl-3-yl-pyrimidin-2-ylamino)-phenyl]-4- chloromethyl benzamide (Imp...
February 27, 2018: Biomedical Chromatography: BMC
Cristina Ioana Stoica, Ioana Ionuț, Laurian Vlase, Brîndușa Tiperciuc, Gabriel Marc, Smaranda Oniga, Cătălin Araniciu, Ovidiu Oniga
No abstract text is available yet for this article.
February 27, 2018: Biomedical Chromatography: BMC
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