QuEchERS-气相色谱-质谱法同时测定果蔬中23种农药残留  

Simultaneous determination of 23 pesticides residues in fruits and vegetables by QuEchERS-gas chromatography-mass spectrometry

作　　者：王海萍[1] 王红玲[1] 陈建文[1] 秦鹏[1] WANG Hal - ping WANG Hong - ling CHEN Jian - wen QIN Peng(Rizhao Center for Disease and Prevention, Rizhao, Shandong 276826, Chin)

机构地区：[1]日照市疾病预防控制中心,山东日照276826

出　　处：《中国卫生检验杂志》2017年第9期1250-1252,1258,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立果蔬中23种农药残留的QuEchERS-气相色谱-质谱分析方法。方法称取经粉碎匀浆后的样品,经酸性乙腈提取,按照QuEchERS试剂盒操作方法,经PSA粉(N-丙基乙二胺)、石墨化碳粉及碳十八粉混合净化后,由DB-1701毛细管柱(30 m×0.32 mm,0.25μm)分离,气相色谱-质谱法测定,峰面积外标法定量。结果该方法23种农药在0.5μg/ml^2.0μg/ml的浓度内线性相关系数(r)均>0.995,方法的检出限(LOD)为0.001 mg/kg^0.025 mg/kg,23种农药的回收率为80.25%~97.78%,相对标准偏差(RSD)为3.83%~12.17%。在所检测的140份果蔬样品中,有9份样品检出克百威、氯氟氰菊酯及敌敌畏等农药残留,其中西红柿样品检出2份氯氟氰菊酯超出国家限量。结论本方法稳定可靠,操作简便快速,方法回收率高,可满足果蔬中23种农药残留的检测要求。Objective To establish a method for the determination of 23 pesticides residues in fruits and vegetables by QuEchERS - gas chromatography/rnass spectrometry. Methods The samples were crushed, homogenated, and then extracted with acidic acetonitrile and purified by PSA, graphitized carbon black and C18 on the basis of QuEchERS kits operation method. Finally, the samples were separated with DB - 1701 column （30 m × 0.32 mm, 0.25μm） and determined by gas chromatography - mass spectrometry. Peak area external standard method was used for quantification. Results The correlation coefficients （r） were greater than 0. 995 when the concentrations of 23 pesticides were within 0.5 μg/ml - 2.0μg/ml. The detection limits were within 0.001 mg/kg-0. 025 mg/kg and the recovery rates were within 80.25% -97.78%. The relative standard deviations （RSDs） were within 3.83% - 12.17%. Among the 140 samples of fruit and vegetable tested, pesticide residues such as carbu- thran, cyhalothrin and dichlorvos were tested in 9 samples, and the cyhalothrin was detected in 2 tomatoes copies, which was beyond national limits. Conclusion The method is stable, reliable, simple, rapid, and has a high recovery rate, which can be applied for the determination of 23 kinds of pesticides residues in fruits and vegetables.

关 键 词：QUECHERS 气相色谱-质谱法 农药残留 果蔬 

分 类 号：O657.63[理学—分析化学]