摘要
目的建立LC-MS/MS测定人血浆中罗红霉素浓度的方法,并研究其制剂的生物等效性。方法以克拉霉素为内标,色谱柱:Alltech Alltima(2.1 mm×100 mm,3.5μm);流动相:0.1%甲酸溶液-乙腈(45∶55);流速:0.2 mL·min-1;柱温:30℃。采用三重四极杆串联质谱,电喷雾离子源,正离子模式检测,以选择反应监测(SRM)方式进行检测,罗红霉素母离子[M+H]+m/z 837.5,子离子m/z 679.2,内标克拉霉素母离子[M+H]+m/z 748.5,子离子m/z 590.2。结果罗红霉素线性范围为0.10～20.00μg·mL-1,最低检测限为0.01μg·mL-1,3种浓度的相对回收率为100.8%～103.1%,日内、日间RSD均<5.9%(n=5)。生物等效性研究表明受试制剂和参比制剂生物等效,受试制剂相对生物利用度为(100.655±9.552)%(P=0.5%)。结论该方法专属、灵敏、快速,适用于罗红霉素制剂的生物等效性研究。
OBJECTIVE To establish a LC-MS/MS method for determination of roxithromycin in plasma and to study its bioequivalence. METHODS Clarithromycin was used as internal standard. The method was performed on Alltech AUtima （2.1 mm×100 mm, 3.5 μm） at 30℃, and 0.1% formic acid-acetonitrile（45 ： 55） was used as mobile phase with the flow rate of 0.2 mL.min^-1. Electrospray ionization source was applied and operated in positive ion mode. Selected reaction monitoring（SRM） mode with the transitions of m/z 837.5→679.2 and m/z 748.5→590.2 was used to quantify roxithromycin and clarithromycin, respectively. RESULTS The assay was linear over the range of 0.10-20.00 μg.mL^-1, the limit of detection was 0.01 μg.mL^-1, relative recoveries at three level concentrations ranged from 100.8% to 103.1% , the intra- and inter-day precision（RSD） were below 5.9%. Bioequivalence study showed the test roxithromycin tablets was bioequivalent to the reference tablets. The relative bioavailability of the test sample was （100.655±9.552）%（P=0.5%）. CONCLUSION The method is simple, rapid, accurate and can be applied to perform the bioequivalence research of roxithromycin tablets.
出处
《中国现代应用药学》
CAS
CSCD
2012年第12期1128-1131,共4页
Chinese Journal of Modern Applied Pharmacy
