摘要
目的 建立HPLC-MS法测定氯酚伪麻缓释片中对乙酰氨基酚的血药浓度。方法 以盐酸纳洛酮为内标，血浆经甲醇沉淀蛋白后，取上清液进行HPLC-MS法分析。采用Lichrospher C18（250mm×4．6 mm，5／μm，ID）柱进行分离；甲醇-40 mmol·L^-1醋酸铵缓冲溶液（含0.05％的甲酸）（55：45，v／v）为流动相；检测离子为对乙酰氨基酚m／z：152．2、内标m／z：328．2；裂解电压为70V。结果 血浆中杂质不干扰样品的测定，在0．03012～12．05μg·ml^-1范围内线性关系良好，最低定量限为0．03012μg·ml^-1；高、中、低3种浓度的日间和日内变异均小于11．0％；绝对回收率在91．4％～93．8％；相对回收率在103．3％-108．9％。结论 本实验所建立的HPLC-MS分析方法，快速、灵敏、准确、简便，符合生物样品分析要求。
AIM To develop an HPLC-MS for the determination of paracetamol in the plasma of volunteers who administrated the compound sustained-release tablet of loratadine, paracetamol and pseudoephedrine sulfate. METHODS After being deproteinized with methanol,the supplements were separated on a C18 column with a mobile phase consisted of 55% of methanol and 45% of 40 mmol· L^-1 ammonium acetate buffer containing 0.05% formic acid. Naloxone hydrochloride was used as the internal standard（IS）. The flow rate of the mobile phase was 1 ml· min^- 1. The instrument was run in the selected ion monitoring （SIM） mode with the target ions of m/z ： 152.2 for paracetamol, and m/z：328.2 for the IS. RESULTS Calibration curve for paracetamol was linear over the range of 0.03012 - 12.05 μg· ml^-1. The lower limit of quantitation was 0.03 gg＇ ml- 1. The recovery was 91.4 % - 93.8 %. The intra and inter-run precision was less than 11%. CONCLUSIONS The assay was proved to be sensitive,accurate and convenient. It can be applied to study the plarmacokinetics of paracetamol in humans.
出处
《江苏药学与临床研究》
2006年第6期381-383,共3页
Jiangsu Pharmacertical and Clinical Research
