液相色谱-串联质谱法测定人血浆中克林霉素

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 ×2.0 mm×5 μm），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/z 425.2→126.3（克林霉素）和 m/z 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>0.99），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。

Determination of Clindamycin in Human Plasma by LC-MS/MS

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.