高效液相色谱-串联质谱法测定香菇中23种有机磷农药.PDF

※分析检测 食品科学 2014, Vol.35, No.04 159 高效液相色谱-串联质谱法测定香菇中 23 种有机磷农药 梁达清，苏肯明，张菊梅，郭伟鹏 （广东省微生物研究所，省部共建华南应用微生物国家重点实验室（省部共建国家重点实验室培育基地），广东省微生物应 用新技术公共实验室，广东省微生物分析检测中心，广东 广州 510070 ） 摘  要：采用高效液相色谱- 串联质谱法测定香菇中23 种有机磷农药残留。样品通过乙腈提取、盐析分配，得 N 到的乙腈提取液采用C 18和 -丙基乙二胺粉末分散固相萃取净化，经高效液相色谱- 串联质谱仪分析，采用电喷 雾正离子方式及多反应监测模式测定，基质匹配标准溶液外标法定量。方法的定量限达到0.01 mg/kg ；回收率为 70.2%～105.0%，相对标准偏差为3.5%～13.0%。该方法灵敏、准确、快速，可满足香菇中多种有机磷农药残留的 检测要求。 关键词：高效液相色谱- 串联质谱法；有机磷农药；残留；香菇 Determination of 23 Organophosphorus Pesticide Residues in Lentinus edodes by High Performance Liquid Chromatography-Tandem Mass Spectrometry LIANG Da-qing, SU Ken-ming, ZHANG Ju-mei, GUO Wei-peng (State Key Laboratory of Applied Microbiology, Ministry-Province Jointly Breeding Base, South China, Guangdong Provincial Open Laboratory of Applied Microbiology, Guangdong Detection Center of Microbiology, Guangdong Institute of Microbiology, Guangzhou 510070, China) Abstract: A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) method was established for the determination of 23 organophosphorus pesticide residues in Lentinus edodes. Samples were extracted with acetonitrile and separated by salting out method, and then the supernatants were purified using dispersive solid-phase extraction (C18 and primary-secondary amine powder) prior to HPLC-MS-MS analysis. The analytes were identified in positive electrospray ionization and multiple reaction-monitoring modes. The matrix-matched external standard calibration curves were used for quantitative analysis. Under the optimal conditions, the limit of quantitation of the method w