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加速溶剂萃取结合气相色谱-三重四极杆质谱测定枸杞中有机磷农药多残留
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作者单位
冯春,石志红,吴兴强,胡雪艳,范春林 1.河北大学化学与环境科学学院2.中国检验检疫科学研究院 
基金项目:特色高值农产品新型甄别检测关键技术研究(2017YFF0211300)
中文摘要:建立了加速溶剂萃取与气相色谱-三重四极杆质谱联用(GC-MS/MS)法对枸杞中20种有机磷农药残留进行测定。样品经酸化乙腈-二氯甲烷(体积比4∶1)提取,Cleanert TPH固相萃取柱净化,旋转蒸发浓缩后氮吹至干,采用GC-MS/MS检测,并对萃取溶剂、温度、冲洗体积等实验条件进行了优化。结果表明,20种药物在1~500 μg/kg范围内线性良好,相关系数(r2)为0.999 0~0.999 8;在20、40、100 μg/kg 3个加标水平下的回收率为70.0%~82.9%,相对标准偏差(RSD,n=5)为0.6%~8.5%,定量下限为1~15 μg/kg。该方法样品前处理简单、定量准确,适用于枸杞中有机磷农药残留的检测。
中文关键词:加速溶剂萃取  有机磷农药  固相萃取(SPE)  气相色谱-三重四极杆质谱
 
Determination of Organophosphorus Pesticide Residues in Chinese Wolfberry by Gas Chromatography-Triple Quadrupole Mass Spectrometry with Accelerated Solvent Extraction
Abstract:A gas chromatography triple quadrupole mass spectrometry(GC-MS/MS) with accelerated solvent extraction was developed for the determination of 20 organophosphorus pesticides residues in Chinese wolfberry.The samples were first extracted with acidified acetonitrile-dichloromethane(4∶1,by volume),then purified on a Cleanert TPH solid phase extraction column,next concentrated by rotary evaporation and dried with nitrogen,and finally analyzed by GC-MS/MS.The experimental conditions such as extraction solvent,temperature and rinse volume were optimized.Results showed that the calibration curves for 20 pesticides were linear in the range of 1-500 μg/kg with their correlation coefficients(r2) of 0.999 0-0.999 8.The spiked recoveries at three levels of 20,40 and 100 μg/kg were in the range of 70.0%-82.9% with the relative standard deviations(RSDs,n=5) of 0.6%-8.5%.The limits of quantitation of the method ranged from 1.0 μg/kg to 15.0 μg/kg.The method is simple and accurate,and is suitable for the determination of organophosphorus pesticide residues in Chinese wolfberry.
Key Words:accelerated solvent extraction  organophosphorus pesticides  solid phase extraction(SPE)  gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS)
引用本文:冯春,石志红,吴兴强,胡雪艳,范春林.加速溶剂萃取结合气相色谱-三重四极杆质谱测定枸杞中有机磷农药多残留[J].分析测试学报,2019,(4):417-422.
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