title: Optimization of solid-phase extraction and liquid chromatography-tandem mass spectrometry for simultaneous determination of capilliposide B and its active metabolite in rat urine and feces: Overcoming nonspecific binding.
abstract: Capilliposide B, a novel oleanane triterpenoid saponin isolated from Lysimachia capillipes Hemsl, showed significant anti-tumor activities in recent studies. To characterize the excretion of Capilliposide B, a reliable liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for simultaneous determination of Capilliposide B and its active metabolite, Capilliposide A in rat urine and feces. Sample preparation using a solid-phase extraction procedure was optimized by acidification of samples at various degrees, providing extensive sample clean-up with a high extraction recovery. In addition, rat urinary samples were pretreated with CHAPS, an anti-adsorptive agent, for overcoming nonspecific analytes adsorption during sample storage and process. The method validation was conducted over the curve range of 10.0-5000ng/ml for both analytes. The intra- and inter-day precision and accuracy of the QC samples showed ≤11.0% RSD and -10.4-12.8% relative error. The method was successfully applied to an excretion study of Capilliposide B following intravenous administration.
authors: School of Pharmacy, Weifang Medical University, 7166 Baotong West Street, Weifang, Shandong 261053, China.
authors: Zhongzhe
authors: Z
authors: Cheng
authors: Tongji School of Pharmacy, Huazhong University of Science and Technology, 13 Hangkong Road, Wuhan, Hubei 430030, China.
authors: Xing
authors: X
authors: Zhou
authors: Tongji School of Pharmacy, Huazhong University of Science and Technology, 13 Hangkong Road, Wuhan, Hubei 430030, China.
authors: Wenyi
authors: W
authors: Li
authors: Tongji School of Pharmacy, Huazhong University of Science and Technology, 13 Hangkong Road, Wuhan, Hubei 430030, China.
authors: Bingying
authors: B
authors: Hu
authors: Department of Pharmacy, Tongji Hospital of Tongji Medical College, Huazhong University of Science and Technology, 13 Hangkong Road, Wuhan, Hubei 430030, China.
authors: Yang
authors: Y
authors: Zhang
authors: Medical Research Center, Humanwell Healthcare (Group) Co., Ltd, 666 Gao xin Road, Wuhan, Hubei 430075, China.
authors: Yong
authors: Y
authors: Xu
authors: Department of Biomedical Engineering, Zhejiang University, Hangzhou 310027, Zhejiang, China. Electronic address: zhanglin@zju.edu.cn.
authors: Lin
authors: L
authors: Zhang
authors: Tongji School of Pharmacy, Huazhong University of Science and Technology, 13 Hangkong Road, Wuhan, Hubei 430030, China. Electronic address: jianghongliang@hust.edu.cn.
authors: Hongliang
authors: H
authors: Jiang
mesh_terms: D000818:Animals; D002853:Chromatography, Liquid / Q000379:methods; D005243:Feces / Q000737:chemistry*; D005260:Female; D008297:Male; D011485:Protein Binding / Q000502:physiology; D051381:Rats; D017207:Rats, Sprague-Dawley; D012503:Saponins / Q000032:analysis* / Q000378:metabolism* / Q000652:urine; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014315:Triterpenes / Q000032:analysis* / Q000378:metabolism* / Q000652:urine
chemical_list: D012503:Saponins; D014315:Triterpenes; C511099:capilliposide B
keywords: Capilliposide B; Excretion; LC–MS/MS; Nonspecific binding