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Biomedical Chromatography: BMC

Narayan Balaji, Bhavesh Babulal Gabani, Umesh Todmal, Suresh P Sulochana, Neeraj Kumar Saini, Rajesh Chandran, Ramesh Mullangi
We developed and validated a simple, sensitive, selective and reliable LC-MS/MS-ESI method for direct quantitation of dropropizine enantiomers namely levodropropizine (LDP) and dextrodropropizine (DDP) in rat plasma without a need of derivatization as per regulatory guideline. Dropropizine enantiomers and carbamazepine (internal standard; IS) were extracted from 50 μL rat plasma using ethyl acetate. LDP and DDP resolved with good baseline separation (Rs = 4.45) on a Chiralpak IG-3 column. The mobile phase consisted of methanol with 0...
November 13, 2018: Biomedical Chromatography: BMC
Takeo Yasu, Kenji Momo, Hiroshi Yasui, Seiichirou Kuroda
Ibrutinib is an oral inhibitor of Bruton tyrosine kinase, which is one of the key drugs used for the treatment of chronic lymphocytic leukemia (CLL) and mantle cell lymphoma (MCL). In this study, we aimed to develop a simple method for determining plasma ibrutinib concentration. The analysis required extraction of a 200 μL plasma sample and precipitation of proteins using solid-phase extraction. Ibrutinib and nilotinib, which was used as an internal standard, were separated using high-performance liquid chromatography (HPLC) using a mobile phase of acetonitrile:0...
November 13, 2018: Biomedical Chromatography: BMC
Ya-Xin Zhao, Meng Wang, Wan-Ting Dong, Yang Li
A highly sensitive and selective method based on ultra-high performance liquid chromatography combined with linear ion trap-Orbitrap tandem mass spectrometry (UHPLC-LTQ-Orbitrap-MS) has been developed and validated for the determination of scopoletin in dog plasma. The analyte was extracted from plasma samples by using acetonitrile and separated on an ACQUITY UPLC BEH C18 column (50 × 2.1 mm, 1.7 μm) with 0.05% ammonium hydroxide and acetonitrile as mobile phase. The developed method was linear over the concentration range of 1-500 ng/mL, with a correlation coefficient more than 0...
November 13, 2018: Biomedical Chromatography: BMC
Shuang Bai, Pei Li, Jing Liu, Can Cui, Qing Li, Kaishun Bi
To explore whether alcohol has an effect on the pharmacokinetic behavior of phenolic acids, the main bioactive constituents in red wine, a highly sensitive and simple ultra-fast liquid chromatography coupled with triple quadrupole mass spectrometry (UFLC-MS/MS) method was developed for simultaneous quantitation of eight phenolic acids in plasma samples. Plasma samples were extracted by liquid-liquid extraction and the chromatographic separation was achieved on a ZORBAX SB-C18 column within 7.0 min. Results of the validated method revealed that all the calibration curves displayed good linear regression (r > 0...
November 13, 2018: Biomedical Chromatography: BMC
M H Cháirez-Ramírez, J A Gallegos-Infante, M R Moreno-Jiménez, R F González-Laredo, N E Rocha-Guzmán
Lupeol is a dietary triterpene that shows limited water solubility, which affects its bioavailability. It is well known that poor oral bioavailability is one of the major causes of therapeutic variability. Lupeol has been reported with multiple biological activities; however, there are no reports about its bioavailability. Therefore, the objective of this research was to evaluate the systemic bioavailability of lupeol. An experimental strategy with three groups of female CD-1 strain mice was proposed (control, olive oil and lupeol in olive oil), at six experimental times (0...
November 12, 2018: Biomedical Chromatography: BMC
Yuanyuan Ge, Zhen Li, Lu Zhang, Jin Li, Jun He, Jia Hao, Xiu-Mei Gao, Yan-Xu Chang
A sensitive and accurate LC-MS/MS method was established for quantifying bisabolangelone in rat plasma and tissues. Bisabolangelone was isolated and purified from Angelicae pubescentis radix. The pharmacokinetic and tissue distribution of bisabolangelone after administration to rat was performed by LC-MS/MS. Separation was carried out on C8 (4.6 × 100 mm, 1.8 μm) column. The MS/MS transitions of bisabolangelone and tussilagone (internal standard) were set at m/z 249.1→109.1 and m/z 391.4→217.4, respectively...
November 9, 2018: Biomedical Chromatography: BMC
Siva Sankara Rao Yadlapalli, Vijaya Kumari Karra, Vinutha Kommineni, Naresh Kumar Katari, Surendra Babu Manabolu
A highly sensitive, specific and rapid Liquid Chromatography-Tandem Mass Spectrometry technique for the quantification of tasimelteon in human plasma has been developed and validated using tasimelteon-d5 as internal standard. Liquid- liquid extraction technique with ethyl acetate was used for extraction of tasimelteon from the plasma. The chromatographic separation was achieved on Agilent Zorbax, Eclipse, C18, (4.6*50 mm, 5μm) column using the mobile phase of acetonitrile and 0.02% formic acid buffer (85:15, v/v) with the flow rate of 0...
November 9, 2018: Biomedical Chromatography: BMC
Poonam Giri, Nirmal Patel, Vipul Joshi, Shyamkumar Giri, Nuggehally R Srinivas
Bioanalysis plays a key role during drug discovery process to generate the pharmacokinetic data to facilitate unbiased evaluation of leads, optimized leads and drug candidates. Such pharmacokinetic data are used to enable key decisions in the drug discovery process. The aim of the work is to put forward a new strategy of performing the incurred sample reanalysis (ISR) for select small molecule Novel Chemical Entities (NCEs) at different stages of drug discovery prior to candidate selection. Three discovery programs representing hits, leads and optimized lead candidates were selected for the ISR analysis...
November 9, 2018: Biomedical Chromatography: BMC
Giacomo Russo, Francesco Barbato, Damiano Gustavo Mita, Lucia Grumetto
A quick and inexpensive validated method, based on sample treatment by liquid-liquid microextraction followed liquid chromatography (LC) coupled with ultraviolet tandem fluorescence detection, is here proposed for the determination of fifteen multiclass pollutants both in serum and in saliva, a simple and easy to draw matrix. The method was set up and validated according to European guidelines. The compounds of interest include some endocrine disrupting chemicals (i.e. bisphenol A, bisphenol B, bisphenol E, bisphenol F, bisphenol AF, bisphenol A diglycidyl ether, bisphenol M, diethylhexyl phthalate, monoethylhexyl phthalate, triclosan, 4-nonylphenol), as well as other pollutants belonging to the class of volatile organic compounds (2-chlorophenol, 1,2 dichlorobenzene, 1,2,4,5-tetrachlorobenzene)...
November 8, 2018: Biomedical Chromatography: BMC
Mingyu Duan, Qi Zhao, Dafang Zhong, Yue Yuan
AIM: To study pharmacokinetics of R-(-)ondansetron (R-ond) compared with that of S-(-)ondansetron (S-ond) in rats. METHODS: After R-ond and S-ond were injected intravenously into rats at a dose of 2.0 mg/kg, respectively. Stability of ondansetron enantiomers in rat were determined by chiral HPLC, and the concentrations of R-ond and S-ond in plasma were determined by an LC/MS/MS method. The pharmacokinetic parameters were calculated and analyzed statistically using the t test...
November 8, 2018: Biomedical Chromatography: BMC
Haiping Wang, Liguo Zheng, Wanting Yu, Xiaomin Cao, Renbin Yang
As chlorpyrifos is used globally to control pests in sugarcane fields, analysis of its residues on food crops is essential to assess products safety for human being. In this study, chlorpyrifos content in sugarcane plants, soil and juice were determined using a gas chromatography with an electron capture detector. The limit of quantification was 0.01 mg/kg for plant and soil, 0.01 mg/L for juice. The degradation and residual risk in sugarcane fields after applying chlorpyrifos to two sample sites (Changsha and Danzhou, China) were assessed...
November 7, 2018: Biomedical Chromatography: BMC
Ying Lu, Huiyu Yan, Shiyong Teng, Xige Yang
A simple and sensitive liquid chromatography-tandem mass spectrometry method was developed for the simultaneous determination of chebulinic acid and chebulagic acid in rat plasma and tissues and well used in the pharmacokinetic and tissue distribution studies after intraperitoneal injection administration. Samples were processed with methanol by, and chromatographic separation was performed on an Agilent ZORBAX SB-C18 column (50 mm × 2...
November 5, 2018: Biomedical Chromatography: BMC
Feifei Nong, Zhongxiang Zhao, Xia Luo, Chang Liu, Hui Li, Qi Liu, Bin Wen, Lian Zhou
Dahuang-mudan decoction (DMD) has been widely used for disease treatment in China for 1700 years. The formula consists of Rhubarb, Moutan bark, Prunus persica, Wax gourd kernel and Mirabilite, which have been well studied by multidisciplinary approaches. However, the role of the mineral Mirabilite in DMD is unclear. The objective of this study was to investigate the effects of Mirabilite on the absorption and pharmacokinetics of the ingredients in DMD. The constituents were identified in DMD extract and the plasma of Mirabilite-DMD (MDMD, 50 g kg-1 )-treated rats and None Mirabilite-DMD (NMDMD, 50 g kg-1 )-treated rats...
October 31, 2018: Biomedical Chromatography: BMC
Ye Xu, Xiaoyan Chen, Dafang Zhong
Triptolide is one of the main active ingredients of Tripterygium wilfordii Hook. F. In this study, a sensitive LC-MS/MS method was established and validated to determine the concentration of triptolide in rat plasma. Triptolide and an internal standard ((5R)-5-hydroxytriptolide) were extracted from 100 μL of rat plasma with acetonitrile, and the dried residue was then reconstituted and reacted with benzylamine to produce benzylamine triptolide and benzylamine (5R)-5-hydroxytriptolide. Derivatization increased the sensitivity of triptolide detection by approximately 100-fold...
October 29, 2018: Biomedical Chromatography: BMC
Kai Niu, Huiyu Yan, Chunjie Guo, Sixi Zhang, Wei Zhu, Shiyong Teng
A highly sensitive LC-MS/MS method was developed to measure oroxin B in rat plasma and tissue homogenates. The analyte and IS were isolated from biological matrices by a simple protein precipitation followed by centrifugation. Detection was conducted by electrospray negative-ionization mass spectrometry in selected-reaction monitoring mode. The assay was linear in the concentration range 4.52-904 ng/mL with intra- and inter-day precision of <14.41%. It was successfully applied to the pharmacokinetics and tissue distribution studies of oroxin B after an intravenous dose of 1...
October 27, 2018: Biomedical Chromatography: BMC
Victor Pena Ribeiro, Caroline Arruda, Jonas Joaquim Mangabeira da Silva, Jennyfer Andrea Aldana Mejia, Niege Araçari Jacometti Cardoso Furtado, Jairo Kenupp Bastos
Copaifera is a tree that produces an oleoresin that has great historical and economic importance. These oleoresins display several pharmacological properties, such as anti-inflammatory and antimicrobial, among others. The commercialization of Copaifera oleoresin occurs, in many cases, without any quality control, which facilitates its adulteration. Validated analytical methods can provide a safely quality control. In this work, the 800 automatic spinning band distillation equipment was used to perform the fractionation of the volatile oils obtained by hydrodistillation of Copaífera multijuga, C...
October 26, 2018: Biomedical Chromatography: BMC
Zhongrui Liu, Liwen Sun, Hong Yang, Xin Zheng, Libo Wang
Bisphenol A (BPA) is a common additive in food packaging materials, and many methods have been discovered to limit BPA for the sake of food safety. This study aims to find a more sensitive quantification method for BPA. It was determined that a diazo derivative of BPA could be obtained when reacted with a stable and inexpensive reagent, p-methylaniline, exhibiting an increased response in the ultraviolet spectrum than that of non-reacted BPA. Based on this discovery, an accurate method of BPA quantitation was established using a precolumn derivatization HPLC method...
October 26, 2018: Biomedical Chromatography: BMC
Jianbo Li, Yue Jin, Huiyan Fu, Yihui Huang, Xianqin Wang, Yunfang Zhou
Gelsenicine was one of indole alkaloids isolated Gelsemium elegans Benth. In recent years, the role of Gelsemium elegans Benth preparations in anti-tumor, analgesic, dilatation and dermatological treatment has attracted attention, and it has been applied clinically, but it is easy to cause poisoning. An UPLC-MS/MS method was established to determine the gelsenicine in the mouse blood, and the pharmacokinetics of gelsenicine after intravenous (0.1 mg/kg) and intragastric (0.5, 1 mg/kg) administration was studied...
October 26, 2018: Biomedical Chromatography: BMC
Xueting Yao, Yang Liu, Ling Song, Ji Jiang, Fei Xiao, Dongyang Liu, Pei Hu
A simple high performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS) method was developed and fully validated to simultaneously determine teriflunomide (TER) and its metabolite 4-trifluoro-methylaniline oxanilic acid (4-TMOA) in human plasma and urine. Merely 50 μL plasma and 20 μL urine were employed in sample preparation using protein precipitation and direct dilution method, respectively. Agilent Zorbax eclipse plus C18 column was selected to achieve rapid separation for TER and 4-TMOA within 3 min...
October 26, 2018: Biomedical Chromatography: BMC
Chang-Shun Liu, Xiao Liang, Xiao-Han Wei, Fei-Long Chen, Qing-Fa Tang, Xiao-Mei Tan
Diarrhoeal diseases alter the composition of intestinal flora, thereby affecting the efficacy of herbal medicinal formulations. Gegen Qinlian decoction (GQD), a Chinese traditional herbal formulation, is widely used to treat infectious diarrhoea. However, little is known about the microbial disposition of GQD in diarrhoeal state. In this study, the comparative metabolism of components of GQD by diarrhoeal and normal intestinal flora was investigated in vitro. UPLC-MS/MS was performed for simultaneous analysis of eight ingredients of GQD in bacterial solution...
October 26, 2018: Biomedical Chromatography: BMC
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