健康人血浆中伪麻黄碱浓度的LC-MS法测定

Determination of pseudoephedrine in human healthy volunteers′ plasma by LC-MS

目的建立人血浆中伪麻黄碱的LC—MS测定法。方法血浆中加入内标格列吡嗪，用甲醇提取后，采用选择性离子检测（SIM）方法测定其血药浓度。10名健康受试者口服受试制剂后，用LC—MS测定血浆中伪麻黄碱浓度。色谱柱：XTerra MS C18（3．5μm×100mm×2．1mm）；流动相：甲醇-5mmol·L^-1的醋酸铵水溶液（90：10，v／v）；流速：0．2ml·min^-1；柱温：25℃。结果标准曲线线性范围为5．01～1002．00μg·L^-1，标准曲线线性关系良好，回归方程为：f=0．00332×C＋0．00088（r=0．9997，n=5），定量下限为（LLOQ）为5．01μg·L^-1。高、中、低三种浓度的日内和日间变异均小于10．0％，回收率在89．6％～95．1％。结论本方法操作简便，灵敏度高，样品稳定性良好，适用于伪麻黄碱的临床血药浓度检测、生物利用度和药代动力学研究。

Aim To establish a sensitive and specific method for determination of pseudoephedrine in human plasma by LC-MS. Methods Pseudoephedrine was extracted from plasma with 0.8 ml methanol, with an addition of glipizide. LC analysis was carried out through XTerra MS C18 column（ 3.5 μm × 100 mm × 2.1 mm ）. The mobile phase consisted of methanol-5 mmol· L^-1 LNHaAC（90： 10,v/v） at a flow rate of 0.2 ml · min^-1. The column temperature is 25 ℃. Analysis in the mass spectrometer was performed in the selectedion monitoring model. 10 healthy volunteers received tested tablets for a single oral close of pseudoephedrine 120 mg. Drug concentrations in plasma were determined. Results The standard curve was linear in the range of 5.01 - 1002.00 μg · L^-1 （f = 0. 003 32 × C ＋ 0. 000 88,r = 0. 999 7, n = 5 ）. The lowest limit of quantitation was 5.01 μg · L^-1. The relative standard derivation of intra-day and inter - day was smaller than 10%. The recoveries of pseudoephedrine were 89.6% - 95.1%. Conclusion The method was specific,sensitive,simple and suitable for determination of pseudoephedrine in human plasma,bioavailability and pharmacokinetics researches.