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