大鼠体内淫羊藿素葡萄糖醛酸代谢物的定量研究  

Quantitative investigation of glucuronidated icaritin metabolite in rats

作　　者：张双庆[1] 孙丽翠[1] 黄振武[1] 

机构地区：[1]中国疾病预防控制中心营养与健康所,北京100050

出　　处：《卫生研究》2015年第1期91-94,共4页Journal of Hygiene Research

摘　　要：目的建立超高效液相色谱一串联质谱法（UHPLC—MS／MS）同时测定大鼠血浆中淫羊藿素（ICT）及其葡萄糖醛酸代谢物（GICT）浓度，并用于定量研究ICT在大鼠体内的代谢。方法采用乙腈提取血浆中ICT和GICT，以香豆雌酚（CMT）为内标，在c，。色谱柱上以乙腈一水一甲酸铵一甲酸梯度洗脱分离；在电喷雾离子化电离源上以选择反应监测方式进行负离子检测，用于定量分析的离子反应分别为m／z367．1—297。1（ICT），m／z543．3_367．1（GICT）和m／z267．0—211．1（CMT）。大鼠腹腔注射10mg／kgICT，采集不同时刻血样并测定ICT和GICT浓度。结果ICT和GICT的线性范围分别为0．2～20ng／ml和2～200ng／ml，定量下限分别为0．2ng／ml和2ng／ml。ICT和GICT的精密度（RSD）在10．3％以内，准确度在95．1％～103．7％，提取回收率为89．1％～92．4％，基质效应为93．2％～104．2％。结论UHPLC—MS／MS法专属性好、准确度高，适用于ICT在大鼠体内代谢研究，2h时GICT达到最大浓度。ICT在大鼠体内迅速代谢成葡萄糖醛酸II相代谢物GICT。Objective To establish an ultra-high performance liquid chromatography- tandem mass spectrometry（UHPLC-MS/MS） method for the simultaneous quantification of icairitin（ICT） and its major metabolite glucuronidated icaritin （GICT） , and investigate metabolism of ICT in rats following a single intraperitoneal administration. MetbodslCT, GICT and an internal standard coumestrol （CMT） were extracted from rat plasma using acetonitrile and separated on a C18 column using a gradient mobile phase of acetonitrile, water, ammonium formate and formic acid. In the negative electrospray ionization mode, selected reaction monitoring of the precursor-product ion transitions of m/z 367.1---~297.1 for ICT, 543.3--~367.1 for GICT and 267.0---~211.1 for CMT was used for the quantification. Plasma was collected for the determination of ICT and GICT after rats were intraperitoneally administered with ICT at a single dose of 10 mg/kg. Results The calibration curves were linear over the concentration range of 0.2 - 20 ng/ml for ICT and 2 -200 ng/ml for GICT with the respective lower limit of quantification at 0. 2 and 2 ng/ml. The intra- and inter-day accuracy values fell in the range of 95. 1 - 103.7% , and precisions were within 10. 3%. Recovery 104.2% , respectively. Conclusion accurate, suitable for the metabolism in rats. and matrix effect were 89. 1 -92.4% and 93.2 - The UHPLC-MS/MS method was specific and study of ICT. ICT was rapidly metabolized to GICT in rats.

关 键 词：淫羊藿素 淫羊藿素葡萄糖醛酸代谢物 超高效液相色谱-串联质谱代谢 

分 类 号：Q591[生物学—生物化学] R446.11[医药卫生—诊断学]