摘要
为了同时监管禽肉中多种类型(四咪唑类、硝基咪唑类、三嗪类、氨基甲酸酯类和有机氮类)抗虫药,提出了题示研究。取已研磨混匀的样品(2±0.01)g,加入5 m L水和10 m L提取剂(由1 m L乙酸、600 m L乙腈和400 m L乙酸乙酯组成),涡旋振荡20 min,加入无水Mg SO40.5 g,离心5 min。取5 m L上层液于40℃氮气吹干,在净化管中加入20 mg C18粉、30 mg N-丙基乙二胺(PSA)粉和1 m L定容液(由1 m L甲酸、900 m L去离子水和100 m L乙腈组成)后涡旋1 min,用0.22μm双系微孔滤膜过滤。以GISTC18-AQ色谱柱(100 mm×2.1 mm,1.9μm)为固定相,以不同体积比的0.1%(体积分数)甲酸溶液-乙腈混合液为流动相梯度洗脱分离滤液中24种抗虫药。质谱分析采用多反应监测模式,基质匹配法定量。结果表明,24种抗虫药的质量浓度在一定范围内与对应的质谱峰面积呈线性关系,检出限(3S/N)为0.01~0.40μg·kg^(-1)。按照标准加入法进行回收试验,回收率为61.2%~113%,测定值的相对标准偏差(n=6)不大于15%。方法用于分析30份实际样品,仅在1份鸭肉样品中检出羟基二甲硝咪唑,检出量为1.46μg·kg^(-1),与农业农村部公告第197号-10-2019、SN/T 4809—2017标准方法中的测定结果基本一致。
A study mentioned by the title was developed for simultaneous monitoring of multiple types of anti-insect drugs(including tetraimidazoles,nitroimidazoles,triazines,carbamates and organic nitrogen pesticides)in poultry meat.The homogenized samples[(2±0.01)g]were taken,and 5 mL of water and 10 mL of extractant solutions,which consisted of 1 mL of acetic acid,600 mL of acetonitrile and 400 mL of ethyl acetate,were added.The mixture was vortexed for 20 min.0.5 g of anhydrous MgSO4 was added and the mixture was centrifuged for 5 min.The supernatant(5 mL)was taken and blown to dryness at 40℃by nitrogen,then vortexed for 1 min after adding 1 mL of solution(consisting of 1 mL of formic acid,900 mL of deionized water,and 100 mL of acetonitrile)and purified by 20 mg of C18 powder and 30 mg of N-propylethylenediamine(PSA)powder in a cleanup tube.The result solution was filtered through a 0.22μm double-layer microfiltration membrane.The 24 anti-insect drugs in filtrate was separated on GISTC18-AQ chromatographic column(100 mm×2.1 mm,1.9μm)as the stationary phase,using the mixtures of acetonitrile and 0.1%(volume fraction)formic acid solution at different volume ratios as the mobile phase for gradient elution.Multiple reaction monitoring mode was adopted in mass spectrometry analysis,with the matrix-matched method for quantification.As shown by the results,linear relationships between the corresponding mass spectrometry peak areas and mass concentrations of 24 anti-insect drugs were found in definite ranges,with detection limits(3S/N)in the range of 0.01—0.40μg·kg^(−1).Test for recovery was made by the standard addition method,giving results in the range of 61.2%—113%,with RSDs(n=6)of the determined values not more than 15%.This method was used to analyze 30 actual samples,and hydroxy dimetridazole was detected in only one duck meat sample with detection amount of 1.46μg·kg^(−1).The results were consistent with those obtained by the standard methods described in Announcement No.197-10-2019 of the Ministry of
作者
王俊燕
郭礼强
田国宁
张金玲
战京芹
WANG Junyan;GUO Liqiang;TIAN Guoning;ZHANG Jinling;ZHAN Jingqin(Animal Disease Prevention and Control Center of Weifang City,Weifang 261041,China;Weifang Customs,Weifang 261041,China;Agricultural Technology Extension Center of Weifang City,Weifang 261041,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2024年第11期1155-1162,共8页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
海关总署科研项目(2021HK200)
潍坊市科学技术发展项目(2020ZJ1323/2021ZJ1133)。
