液相色谱-串联质谱法测定化妆品中的林可霉素等13种抗菌素  

Determination of 13 kinds Antibiotics Lincomycin in Cosmetics by LC-MS/MS

作　　者：叶兰凤[1] 董昌平[1] 叶晓娟[1] 陈丽湘[1] 邱慧珍[1] 

机构地区：[1]福建省南平市药品检验所,南平353000

出　　处：《海峡药学》2013年第11期79-82,共4页Strait Pharmaceutical Journal

基　　金：南平市科技局资助项目(N2012Z26)

摘　　要：目的建立化妆品中林可霉素、氯霉素、庆大霉素、四环素类抗生素及甲硝唑等13种药物的液相色谱．串联质谱检测方法。方法采用40％甲醇溶液提取化妆品中的抗生素，高速冷冻离心处理，经Ultimatex Bc18色谱柱（250mm×4．6mm，5炉1）分离，梯度洗脱，在LC-MS／MS多反应监测（MRM）模式下进行定性及定量分析。其中甲硝唑、林可霉素、庆大霉素、四环素类药物采用正离子扫描模式，氯霉素采用负离子扫描模式。结果除庆大霉素外，其余12种药物的定量限为：0．2～5mg·kg^-1，在0．04～20mg·kg^-1范围内，3个添加水平的平均回收率为76．0％～112．2％，相对标准偏差（RSD，n=6）为4．O％一23．2％。结论该方法可快速、准确地对化妆品中的抗菌药物残留进行定性和定量测定。ABSTRACT ： OBJECTIVE A method for determination of 13 kinds of drugs of lincomycin, chloramphenicol, tetracyclines antibiotics and metronidazole in cosmetics was established by LC-MS/MS. METHODS Sample was extracted with 40% methanol-watersolution, then handled by High-speed refrigerated centrifuge. The chromatographic separation was using C18 column （250mm x 4.6ram,5 Ixm） for gradient elution, then the qualitative and quantitative analysis was carried out with MS/MS （MRM）. Metronidazole, lincomycin, gentamicin and tetracyclines antibiotics were analyzed by positive mode and chloramphenicol was analyzed by negative mode. RESULTS The limits of quantification were 0. 2- 5mg . kg^-1, In the range of 0. 04- 20mg . kg^-1 in three levels, the average recoveries were 76. 0% - 112. 2% ,the relative standard deviations （RSDs） was 4.0%-23.2% of 12 kinds of drugs except gentamicin. CONCLUSION The method was rapid and accurate for the qualitative and quantitative analysis of antibiotics in cosmetics.

关 键 词：液相色谱-串联质谱 林可霉素 氯霉素 四环素 甲硝唑 化妆品 

分 类 号：R927.2[医药卫生—药学]