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首页> 外文期刊>Chromatographia >LC-MS-MS method for simultaneous determination of icariin and its active metabolite icariside II in human plasma
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LC-MS-MS method for simultaneous determination of icariin and its active metabolite icariside II in human plasma

机译：LC-MS-MS法同时测定人血浆中的二十碳素及其活性代谢产物二十碳糖苷II

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摘要

An LC-MS-MS method was revised and validated for simultaneous determination of icariin and its active metabolite icariside II in human plasma. The analytes and daidzein ( IS) were extracted by liquid-liquid extraction and analyzed by LC-MS-MS. The separation was performed by a Zorbax SB-C-18 column (3.5 mu m, 2.1 x 100 mm) with an isocratic mobile phase consisting of methanol-water-formic acid ( 65: 35: 0.035, v/v/v) at a flow rate of 0.25 mL min(-1). Detection was performed on a triple quadrupole tandem mass spectrum by multiple reaction monitoring mode using the electrospray ionization technique in positive mode. The method had lower limits of quantitation 0.2 and 0.1 ng mL(-1) for icariin and icariside II, respectively, using 500 mu L plasma sample. The linear calibration curves were obtained in the concentration range of 0.2-100 ng mL(-1) for icariin and 0.1-100 ng mL(-1) for icariside II. The RSD values of intra- and inter-day precision calculated from quality control ( QC) samples were less than 7.2% for icariin and less than 6.5% for icariside II. The accuracy as determined from QC samples was within 3.8% for each analyte. The method has been applied to determine and evaluate the pharmacokinetic of icariin and its metabolite icariside II in volunteers following oral administration of icariin and extract of Epimedium, respectively.
机译：修改并验证了LC-MS-MS方法，该方法可同时测定人血浆中的icariin及其活性代谢产物icariside II。通过液-液萃取来提取分析物和大豆苷元（IS），并通过LC-MS-MS进行分析。用Zorbax SB-C-18色谱柱（3.5μm，2.1 x 100 mm）进行分离，等度流动相由甲醇-水-甲酸（65：35：0.035，v / v / v）组成流速为0.25 mL min（-1）。使用正离子模式下的电喷雾电离技术，通过多重反应监测模式对三重四极串联质谱进行检测。使用500μL血浆样品时，该方法对大麻素和icariside II的定量下限分别为0.2和0.1 ng mL（-1）。线性校正曲线是在浓度范围为0.2-100 ng mL（-1）时，对ari香素为0.1-100 ng mL（-1）。根据质量控制（QC）样品计算出的日内和日间精度的RSD值，对于icariin小于7.2％，对于icariside II小于6.5％。根据质控样品确定的每种分析物的准确度在3.8％以内。该方法已被应用于分别测定口服和口服淫羊ium苷和淫羊med提取物后志愿者体内的大麻素及其代谢产物柠檬苷II的药代动力学。

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