高效液相色谱-质谱联用法同时测定化妆品中19种喹诺酮类抗生素

Determination of Nineteen Quinolone Antibiotics in Cosmetics by LC-MS/MS

首次建立高效液相色谱-电喷雾电离串联质谱测定化妆品中19种喹诺酮类抗生素的含量分析方法。将不同形态的化妆品样品加入内标后经溶剂超声提取,提取液经高速离心处理,上清液以正己烷脱脂,经0.22μm微孔滤膜过滤后取续滤液,色谱柱为Agilent SB-C18(2.1 mm×100 mm×1.7μm),流动相为质量分数0.1%甲酸水溶液-(体积比85/15)甲醇/乙腈系统梯度洗脱,流速为0.2 mL/min,柱温为30℃,进样量为2μL,经高效液相色谱-电喷雾电离串联质谱测定,内标法定量。19种喹诺酮类抗生素在1~1000 ng/mL的质量浓度范围内呈良好线性关系(相关系数均大于0.995);回收率为85%~115%,相对标准偏差为1.9%~8.9%。各化合物最低检出质量比均为1μg/kg。该方法灵敏度高,重复性好,可用于化妆品中多种喹诺酮类抗生素的检测。

For the first time,an LC-MS/MS method has been developed for the simultaneous determination of nineteen quinolone antibiotics in cosmetics.Different forms of cosmetic samples with internal standard added were prepared by ultrasonic extraction,the extraction solution was obtained by high-speed centrifugation,the supernatant was degreased by hexane,then filtered by 0.22μm millipore filter,and the continued filtrate was taken for analysis.A Waters reversed phase column,Agilent SB-C18(2.1 mm×100 mm×1.7μm)was used with methanol/acetonitrile(volume ratio 85/15)-0.1%(mass fraction)aqueous formic acid as the mobile phase under the condition of gradient elution.When the flow rate was 0.2 mL/min,column temperature was 30℃,the injection volume was 2μL,the samples were determined by high performance liquid chromatography electrospray ionization tandem mass spectrometry,and quantified by internal standard method.The recoveries were 85%-115%with the relative standard deviations of 1.9%-8.9%.All quinolones showed good linearity within the concentration range of 1-1000 ng/mL,the correlation coefficients were greater than 0.995,the detection limits were 1μg/kg.The method has advantages of high sensitivity and good reproducibility,which can be used to detect a variety of quinolone antibiotics in cosmetics.