超高效液相色谱-串联质谱法测定消毒产品中的22种抗生素

目的建立超高效液相色谱-串联质谱法同时检测消毒卫生产品中的5种硝基咪唑类抗生素和17种磺胺类抗生素。方法样品加入混合内标溶液后,经2%甲酸水溶液和乙腈混合溶剂(3∶2,V/V)超声提取,上清液经2%甲酸水溶液稀释后,经MCX固相萃取柱富集净化,2%甲酸水溶液和甲醇溶液分别淋洗,5%氨水甲醇洗脱,洗脱液经氮吹至近干后,1.0 mL 10%甲醇水溶液复溶,经CORTECS^TM UPLC C₁₈(100 mm×2.1 mm, 1.6μm)反相色谱柱分离,超高效液相色谱-串联质谱仪检测分析。结果 22种抗生素在0.05～5.0 ng/mL范围内线性关系良好,相关系数均大于0.999;方法的检出限为0.03～0.15μg/kg,加标回收率为84.3%～121.2%,相对标准偏差为1.13%～8.43%(n=6)。该方法成功用于20份膏霜、水剂型抗(抑)菌消毒产品中违禁抗生素的检测,阳性检出率为45%。结论该方法灵敏度高、选择性好、操作简单,适用于膏霜、水剂型消毒产品中违禁抗生素的检测。

Determination of 22 antibiotics in disinfection products by ultra-performance liquid chromatography tandem mass spectrometry

OBJECTIVE To develop a method for simultaneous determination of 5 nitroimidazole antibiotics and 17 sulfonamides antibiotics in disinfection products by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). METHODS Samples were spiked with isotope internal standard,and then extracted by 2% formic acid solution and aeetonitrile with ultrasonic,followed by MCX column to remove matrix interference and for enrichment.The supernatants were diluted with 2% formic acid solution before loading on the columns,then washed with 2% formic acid solution and methanol respectively,eluted with 5%ammonium methanol.The separation was performed on a CORTECS^TM UPLC C8(100 mm×2. 1 mm,1. 6μm)column by using 0.1%formic acid solution and 0.1% formic acid acetonitrile as mobile phase with gradient elution.The antibiotics were analyzed by UPLC-MS/MS.RESULTS The linear ranges of 22 antibiotics were 0.05-5.0 ng/mL and the correlation coefficients were greater than 0.999.The limits of detection(LODs)were 0.03-0.15 μg/kg and the recoveries were 84.3%-121.2% with the relative standard deviations were 1.13%-8.43%(n=6).The method was successfully used to detect the content of antibiotics in 20 disinfection products,45% of samples had been detected positively.CONCLUSION This method is simple,sensitive,selective and accurate,and could be applied for simultaneous detection of antibiotics in disinfection products.