气相色谱-串联质谱法测定原料类果酱中百菌清残留量  

Determination of chlorothalonil residues in raw jam by gas chromatography-tandem mass spectrometry

作　　者：梁建英 谢瑞龙 胡雪 李慧秀 刘丽君 李翠枝 吕志勇 LIANG Jian-Ying;XIE Rui-Long;HU Xue;LI Hui-Xiu;LIU Li-Jun;LI Cui-Zhi;LV Zhi-Yong(Inner Mongolia Yili Industrial Group Co.,Ltd.,Hohhot 010110,China;Inner Mongolia Yili Industrial Group Co.,Ltd.,Shanghai Branch,Shanghai 200127,China)

机构地区：[1]内蒙古伊利实业集团股份有限公司,呼和浩特010110 [2]内蒙古伊利实业集团股份有限公司上海分公司,上海200127

出　　处：《食品安全质量检测学报》2021年第21期8620-8624,共5页Journal of Food Safety and Quality

摘　　要：目的建立气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)测定原料类果酱中百菌清农药残留的检测方法。方法样品经8 mL去离子水水化,采用乙腈提取,加入4 g氯化钠盐析,4200 r/min离心8 min。上清液经氟罗里硅土固相萃取柱净化,使用正己烷-丙酮混合溶液(9:1,V:V)洗脱,气相色谱-串联质谱仪测定,外标法定量。结果标准曲线在5~250 ng/mL范围内线性良好,相关系数大于0.99。百菌清的定量限为0.01 mg/kg;在0.01~0.10 mg/kg浓度范围的加标实验中,回收率为83.0%~116.8%,精密度为3.7%~10.3%。结论该方法操作简便、结果准确,适用于原料类果酱中百菌清残留的测定。Objective To establish a method for quantitative determination of chlorothalonil pesticide residue in raw jam materials by gas chromatography-tandem mass spectrometry(GC-MS/MS).Methods The sample was hydrated by 8 m L of deionized water,extracted by using acetonitrile,salted out with 4 g sodium chloride,centrifuged at 4200 r/min for 8 min.The supernatant was cleaned up by a florisil solid phase extraction column and eluted by n-hexane-acetone mixture(9:1,V:V),the analytes were determined by GC-MS/MS and quantified by external standard method.Results The standard curve had a good linear relationship in the range of 5-250 ng/m L,with the correlation coefficient was greater than 0.99.The limit of quantification of chlorothalonil was 0.01 mg/kg;the recoveries varied from 83.0%to 116.8%and the relative standard deviations varied from 3.7%to 10.3%at spiked levels of 0.01-0.10 mg/kg.Conclusion This method is simple,convenient,accurate and suitable for detection of chlorothalonil residue in raw jam materials.

关 键 词：原料类果酱 百菌清 农药残留 气相色谱-串联质谱法 

分 类 号：TS255.43[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]