Yu L L, Chao C K, Liao W J, Twu T Y, Liu C M, Yang T H, Lin E T
Department of Pharmaceutical Technology, Mithra Bioindustry Co., Ltd., Taipei Hsien, Taiwan.
J Chromatogr B Biomed Sci Appl. 1999 Mar 19;724(2):287-94. doi: 10.1016/s0378-4347(99)00018-3.
A simple, sensitive and specific liquid chromatography-electrospray tandem mass spectrometry (LC-MS-MS) method for the determination of clindamycin (I) was developed. Both I and verapamil (II, internal standard) were analyzed using a C18 column with a mobile phase of 80% acetonitrile-0.01% trifluoroacetic acid. Column eluents were monitored by electrospray tandem mass spectrometry. Multiple reaction monitoring (MRM) using the parent to daughter combinations of m/z 425-->126 and 455-->165 was used to quantitate I. A limit of quantitation of 0.0500 microgram/ml was found. The assay exhibited a linear dynamic range of 0.0500-20.0 micrograms/ml and gave a correlation coefficient (r2) of 0.998 or better. The chromatographic run time was approximately 2 min. The intra-batch precision and accuracy of the quality controls (QCs, 0.0500, 0.150, 1.50, 15.0 and 20.0 micrograms/ml) were characterized by coefficients of variation (CVs) of 5.13 to 13.7% and relative errors (REs) of -4.34 to 4.58%, respectively. The inter-batch precision and accuracy of the QCs were characterized by CVs of 4.35 to 8.32% and REs of -10.8 to -4.17%, respectively. The method has successfully been applied to the analysis of samples taken up to 12 h after oral administration of 300 mg of I in healthy volunteers.
建立了一种简单、灵敏且特异的液相色谱 - 电喷雾串联质谱法（LC-MS-MS）用于测定克林霉素（I）。I和维拉帕米（II，内标）均使用C18柱进行分析，流动相为80%乙腈 - 0.01%三氟乙酸。柱洗脱液通过电喷雾串联质谱进行监测。采用m/z 425→126和455→165的母离子到子离子组合的多反应监测（MRM）来定量I。定量限为0.0500微克/毫升。该测定法的线性动态范围为0.0500 - 20.0微克/毫升，相关系数（r2）为0.998或更高。色谱运行时间约为2分钟。质量控制品（QCs，0.0500、0.150、1.50、15.0和20.0微克/毫升）的批内精密度和准确度分别以变异系数（CVs）为5.13%至13.7%和相对误差（REs）为 - 4.34%至4.58%来表征。QCs的批间精密度和准确度分别以CVs为4.35%至8.32%和REs为 - 10.8%至 - 4.17%来表征。该方法已成功应用于健康志愿者口服300毫克I后长达12小时采集的样品分析。
