《食品工业》2023年第44卷第2期295分析检测改良QuEChERS-GC-TQT/MS法测定大米中16种有机磷农药残留朱洁灵*，周瑞铮，张树权，莫淑梅，沈昌莹东莞市食品药品检验所（东莞523808）摘要建立同时测定大米中16种有机磷农药残留的QuEChERS-加速溶剂萃取-气相色谱/三重四极杆串联质谱法。称取大米,经加压流体萃取,提取液经无水硫酸钠柱脱水后,旋蒸至近干,加入丙酮溶解后吸取一定样液至多农残净化管中净化,氮吹,丙酮复溶后,供GC-TQT/MS测定。结果表明,16种有机磷农药在质量浓度0.01~1μg/mL的基质曲线范围内呈良好线性关系,相关系数R2大于0.99,在7.5,15和100μg/kg3个浓度水平(n=6)的加标回收率为78.8%~103.8%,相对标准偏差(SRSD)为1.32%~7.78%。方法检出限(SLOD)为2.94~6.83μg/kg,方法定量限(SLOQ)为11.44~14.37μg/kg。该方法具有操作简便、快速高效、回收率高、灵敏度高、重复性好等优点,可用于测定大米中16种有机磷农药残留量。关键词QuEChERS;加速溶剂萃取(ASE);气相色谱/三重四极杆串联质谱法(GC-TQT/MS);大米;有机磷农药Determinationof16OrganophosphorusPesticideResiduesinRicebyModifiedQuEChERS-GC-TQT/MSMethodZHUJieling*,ZHOURuizheng,ZHANGShuquan,MOShumei,SHENChangyingDongguanInstituteforFoodandDrugControl(Dongguan523808)AbstractAQuEChERS-acceleratedsolventextraction-gaschromatography-triplequadrupoletandemmassspectrometrymethodforthesimultaneousdeterminationof16organophosphoruspesticideresiduesinricewasestablished.Thericewasweighedandextractedbypressurizedfluid.Aftertheextractwasdehydratedbyananhydroussodiumsulfatecolumn,itwasrotaryevaporatedtoneardryness.Afterbeingdissolvedinacetone,acertainsamplesolutionwasdrawnintoapesticideresiduepurificationtubeforpurification,afternitrogenblowingandacetoneredissolving,forGC-TQT/MSdetermination.The16organophosphoruspesticidesshowedagoodlinearrelationshipintherangeofthematrixcurvewithaconcentrationof0.01-1μg/mL;ThecorrelationcoefficientR2wasgreaterthan0.99,andthespikedrecoveriesat7.5,15and100μg/kg(n=6)were78.8%-103.8%.Therelativestandarddeviation(SRSD)rangedfrom1.32%to7.78%.Thelimitofdetection(SLOD)were2.94-6.83μg/kg,andthelimitofquantitation(SLOQ)were11.44-14.37μg/kg.Themethodhadadvantagesofsimpleo...
