摘要
在比较不同种类的固相萃取柱净化效果上优化了前处理条件,建立了韭菜基质中58种农药残留的气相色谱-质谱法(GC/MS)检测方法。试样经乙腈提取,采用石墨化炭黑/氨基柱(PC/NH2)净化后,用GC/MS选择离子监测扫描模式(SIM)进行检测,基质匹配溶液外标法定量。结果表明,目标物在65.2~1043.0 ng/mL范围内呈良好的线性相关,相关系数(r)均不小于0.990,方法的检出限(LOD,S/N=3)为0.001~0.007 mg/kg,定量限(LOQ,S/N=10)为0.003~0.024 mg/kg。分别在韭菜基质中做低、中、高3个添加水平的加标回收试验,该方法的平均回收率为62.2%~125.2%,相对标准偏差RSD(n=3)在0.5%~9.5%之间。该方法样品处理简单快速,相比QuEChERS的净化效果要好,灵敏度和选择性高,适用于韭菜复杂基质中多组分农药的筛查确证和定量分析。
To optimize pretreatment conditions in comparing the purification effects of different types of solid phase extraction columns,a gas chromatography-mass spectrometry(GC/MS)method was established for the determination of 58 pesticide residues in chives.The samples were extracted by acetonitrile,cleaned-up with Cleanert PC/NH2 solid-phase extractant,and determined by GC/MS using matrix-matched external standard method.The determination coefficients(R2)of all the 58 pesticides in the range of 65.2~1043.0 ng/mL were not less than 0.990.The limits of detection(LODs)were 0.001~0.007 mg/kg when signal/noise was 3(S/N=3).The limits of quantification(LOQs)were 0.003~0.024 mg/kg(S/N=10).For recovery test,there were three levels(low,medium and high)spiked in chives.The average recoveries of the method were 62.2%~125.2%and the relative standard deviations(RSDs,n=3)were 0.5%~9.5%.Compared with QuEChERS method,the method has the advantages of simple and rapid processing,high purification sensitivity and selectivity which is suitable for screening and quantitative analysis of multi-component pesticides in the chives matrix.
作者
张权
沙比拉·吐拉江
周贻兵
林野
李磊
刘利亚
刘文政
吴玉田
郭华
ZHANG Quan;SHABILA Tu-la-jiang;ZHOU Yi-bing;LIN Ye;LI Lei;LIU Li-ya;LIU Wen-zheng;WU Yu-tian;GUO Hua(Experimental Center,Guizhou Center for Disease Control and Prevention,Guiyang 550004,China;Xinjiang Uygur Autonomous Region Center for Disease Control and Prevention,Urumqi 830002,China)
出处
《食品工业科技》
CAS
北大核心
2019年第20期243-250,261,共9页
Science and Technology of Food Industry
基金
贵州省科技支撑计划(黔科合支撑[2017]2972)
贵州省科技基础条件平台专项计划[黔科合平台人才(2016)5705]
关键词
固相萃取
气相色谱-质谱
农药残留
韭菜
净化效果
solid-phase extraction(SPE)
gas chromatography mass spectrometry(GC/MS)
pesticide residues
chives
purification effect
