液相色谱串联质谱法测定蜂蜜中咪唑类抗生素

Rapid Determination of Nitroimidazoles and Benzimidazoles in Honey Using MFC-LC-MS/MS

采用多次推送过滤净化法-液相色谱-三重四极杆串联质谱法,建立蜂蜜中16种硝基咪唑类和苯并咪唑类抗生素,并对宁夏市售蜂蜜进行分析。样品经乙酸乙酯提取,多层修饰复合纳米材料净化;以乙腈-0.1%甲酸水溶液为流动相,硝基咪唑类和苯并咪唑类抗生素分别用强阳离子交换柱(SCX)和五氟苯基柱(PFP)分离,电喷雾正离子模式进行串联质谱测定。16种硝基咪唑和苯并咪唑类抗生素在0.25~50 ng/mL范围内具有良好线性关系(线性相关系数r≥0.995 0),方法检出限(LOD)和定量限范围分别为0.03~0.5μg/kg和0.1~1.0μg/kg,在3个空白添加浓度(1倍LOQ、2倍LOQ和10倍LOQ)水平下,目标物的平均回收率为80.0%~106.8%,方法精密度(δRSD, n=6)为4.1%~6.7%。试验方法操作快速简单、重现性好,可用于蜂蜜中硝基咪唑类和苯并咪唑类抗生素检测。

It was to develop a rapid method for determination of nitroimidazoles and benzimidazoles in honey by multiplug filtration clean-up-liquid chromatography tandem mass spectrometry(m-PFC-LC-MS/MS) and to provide analytical methodology for the honey in Ningxia province. Honey samples were ultrasonically extracted by buffer solution, cleaned up using column. Nitroimidazoles were separated on NX-SCX chromatographic column and benzimidazoles were separated on NX-PFP chromatographic column with mobile phase of methanol-0.1% formic acid on gradientelution. Ionized by atmospheric pressure chemicalionization, nitroimidazoles and benzimidazoles qualified and quantified using MRM mode of mass spectrometry. The 16 nitroimidazoles and benzimidazoles showed good linear relation in the range of 0.25-50 ng/mL(R≥0.995 0). Average recoveries of nitroimidazoles and benzimidazoles in honey at three spiked levels were 80.0%-106.8% with relative standard deviations from 4.1 to 6.7%. The limit of detection(LOD) and the limit of quantitation(LOQ) for the whole method were 0.03-0.50 μg/kg and 0.1-1.0 μg/kg. The method was accurate, reliable, and could be used as a quality control method for nitroimidazoles and benzimidazoles in honey.