Quantitative determination of helicid in rat biosamples by liquid chromatography electrospray ionization mass spectrometry |
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Authors: | Yuanwei Jia Haitang Xie Guangji Wang Jianguo Sun Wei Wang Huang Qing Xuan Wang Hao Yang Meijuan Xu Yi Gu Chen Yao Jie Shen |
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Institution: | 1. Key Laboratory of Pharmacokinetics and Drug Metabolism, China Pharmaceutical University, 24# Tongjia Xiang Street, Nanjing 210009, China;2. Anhui Provincial Centre for Drug Clinical Evaluation, China;3. Institute of Clinical Pharmacology, Central South University, Changsha, China |
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Abstract: | A simple liquid chromatography electrospray ionization mass spectrometry (LC–ESI–MS) method with highly improved sensitivities for the determination of helicid in rat bile, urine, feces and most tissues was developed. The tissues and feces were firstly homogenized mechanically using deionized water as the media. Bile, urine, tissues and feces homogenates were extracted by liquid–liquid extraction with n-butyl alcohol for sample preparation. The subsequent analysis procedures were performed on a Shimadzu LCMS2010A system (electrospray ionization single quadrupole mass analyzer). A Luna C18 column (150 mm × 2.00 mm, 5 μm) was used as the analytical column, while a mixture of acetonitrile and ammonium chloride water solution was used as the mobile phase. The proportions of mobile phase were changed timely according to gradient programs. Chlorinated adducts of molecular ions M+Cl]? at m/z 319.00 and 363.05 were used to quantify helicid and bergeninum (internal standard), respectively. The method was validated to be accurate, precise and rugged with good linearity. The proposed method was successfully applied to the preclinical tissue distribution and excretion studies of helicid in rats. |
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