摘要:
建立了测定人血浆中克林霉素的LC-MS/MS法.血浆样本用乙腈沉淀蛋白后,选用Shim-pack VP-ODS色谱柱(150 mm X 2.0 mm×5μm),以V(甲醇):V(10 mmol·L~(-1)乙酸铵(含0.25%甲酸))=55:45为流动相,流速为0.4 mL·min~(-1).选用API3200型三重四极杆串联质谱仪的多重反应监测(MRM)扫描方式进行监测,电喷雾离子化源,正离子方式,选择监测离子反应分别为m/g 425.2-126.3(克林霉素)和m/x 256.2→167.3(内标苯海拉明).克林霉素和苯海拉明的保留时间分别为1.77 min和1.79 min;血浆中克林霉素的线性范围为0.030 0～10.0 mg·L~(-1)(r>O.99),定量下限为0.030 0 mg·L~(-1);日内、日间相对标准差(RSD)均小于6%;相对偏差(RE)均在±6%的范围以内;平均提取回收率为(101.1±2.6)%;稳定性试验中,血浆中克林霉素在各种贮存条件下均较稳定.该方法快速、灵敏、专属性强、重现性好,适用于人体内克林霉素的药代动力学研究.
Abstract:
A LC-MS/MS method for determination of clindamycin in human plasma was developed. After protein precipitation with acetonitrile, the analyte and internal standard (I. S. ), diphenhydramine, were separated on a Shim-pack VP-ODS analytical column using the mobile phase of V(methanol) : V(10 mmol · L~(-1) ammonium acetate (containing 0.25 % formic acid)) =55 : 45 at a flow rate of 0.4 mL · min~(-1). Detection was carried out by electrospray positive ionization mass spectrometry in the multiple reaction monitoring (MRM) mode. The MRM transitions of m/z 425.2→126.3 and m/z 256.2→167.3 were used to quantify clindamycin and I. S. , respectively. Clindamycin and I. S. are eluted at 1.77 min and 1.79 min, respectively. The calibration curve is linear over the concentration range of 0. 030 0-10.0 mg · L~(-1) with the lower limit of quantitation (LLOQ) 0.030 0 mg · L~(-1). Inter- and intra-day relative standard deviations are both less than 6%, and the relative errors are within ±6%. The mean extract recoveries are (101.1 ± 2.6)%. In the stability studies, clindamycin in plasma is found to be stable under various storage conditions. It is a rapid, sensitive, selective and reliable method for the determination of clindamycin in human plasma. The method is successfully applied to a pharmacokinetic study in healthy volunteers after oral administration of 300 mg clindamycin.
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