QuEChERS-超滤净化结合GC-QQQ测定酿酒大曲中多种农药残留量  

QuEChERS-application of ultrafiltration combined with GC-QQQ in the determination of multiple pesticide residues in liquor-making Daqu

作　　者：曹栩菡[1] 黄小军 叶麟 潘才惠 CAO Xuhan;HUANG Xiaojun;YE Lin;PAN Caihui(Sichuan Vocational College of Chemical Technology,Luzhou 646000,China;Sichuan National Inspection and Testing Co.Ltd.,Luzhou 646000,China)

机构地区：[1]四川化工职业技术学院,四川泸州646000 [2]四川国检检测有限责任公司,四川泸州646000

出　　处：《食品与发酵工业》2021年第7期238-243,共6页Food and Fermentation Industries

摘　　要：酿酒过程中曲药使用比例较高,曲药中的农药残留可能会部分迁移至酒中,大曲中农药残留量的高低会影响成品酒中的农药残留量。实验采用超滤净化结合气相色谱-三重四级杆质谱法(ultrafiltration purification combined with-chromatography triple quadrupole mass spectrometry,GC-QQQ)对酿酒大曲中可能存在的23种有机磷农药进行同时检测。样品经乙腈提取,QuEChERS-超滤净化后进行GC-QQQ测定。结果表明:在10~100μg/L范围内,23种农药的质量浓度与其峰面积间呈良好的线性关系,相关系数均大于0.999;三水平试验回收率在85%~106%,相对标准偏差均小于10%;23种农药的检出限和定量限分别在0.002~0.035和0.007~0.118 mg/kg。该方法简单、快速、重现性好、稳定性高,可满足酿酒大曲中23种农药残留的检测要求。High dosage of Daqu used in the winemaking process will lead to pesticide residues in it partially migrate to the wine.Thus contributes to the level of pesticide residues in the finished wine.This study was carried out to realize a simultaneous determination of 23 organophosphorus pesticides in liquor-making Daqu by ultrafiltration combined with gas chromatography-triple quadrupole mass spectrometry(GC-QQQ).The samples were extracted by acetonitrile,followed by QuEChERS--ultrafiltration,and then determination by GC-QQQ.According to the results,there was a good linear relationship between the mass concentration and peak area of the 23 pesticides within the range of 10-1000μg/L,with the correlation coefficient(R)of greater than 0.999.Furthermore,at three addition levels,the rate of recovery of sample addition ranged from 85%to 106%,and the relative standard deviations were all less than 10%.Besides,the limits of detection and quantitation of the 23 pesticides were 0.002-0.035 mg/kg and 0.007-0.118 mg/kg,respectively.To sum up,the proposed method in our study is simple and rapid in operation with good reproducibility and high stability,which can meet the detection requirement of 23 pesticide residues in liquor-making Daqu.

关 键 词：超滤净化 气相色谱-质谱法 酿酒大曲 有机磷农药 农药残留 

分 类 号：O657.63[理学—分析化学] TS262.3[理学—化学]