气相色谱-负化学电离源-飞行时间质谱筛查和定量测定天然香精中3种农药残留  

Screening and Determination of 3 Pesticide Residues in Natural Flavoring by Gas Chromatography-negative Chemical Ionization-time of Flight Mass Spectrometry

作　　者：司晓喜 张凤梅 刘志华 陆舍铭 陈进雄 邹楠 李响丽 刘春波 朱瑞芝 

机构地区：[1]云南中烟工业有限责任公司技术中心云南省烟草化学重点实验室,云南昆明650231

出　　处：《化学试剂》2016年第12期1191-1195,共5页Chemical Reagents

基　　金：云南中烟工业有限责任公司技术中心科技资助项目(S-6013047)

摘　　要：为了快速筛查和定量检测天然香精中的农药残留,建立了香精中3种农药的气相色谱-负化学电离源-飞行时间质谱（GC-NCI-TOFMS）分析方法。优化了样品萃取、净化条件以及气相色谱和飞行时间质谱分析条件。样品以V（正己烷）∶V（乙酸乙酯）=1∶1为溶液,超声萃取30 min,萃取液经弗罗里硅土固相萃取柱净化后,进行检测分析。根据特征离子的精确质量数、氯同位素离子峰簇、碎片离子丰度比、保留时间对目标物进行定性鉴定,内标法进行定量测定。3种农药的线性相关系数均大于0.998 6,相对标准偏差〈4.5%,检出限为0.14-0.21μg/kg,3种农药的加标回收率为87%-107%。该方法简单快速、准确性高、灵敏度好,适用于香精中农药残留的快速筛查和定量检测。In order to rapidly screen and determine pesticide residues in natural flavoring,a method was developed for the determination of 3 pesticide residues in flavoring by gas chromatography-negative chemical ionization-time of flight mass spectromery（ GCNCI-TOFMS）. The extraction and purification method of flavoring samples,the chromatogphic condition and TOFMS condition of analysis were critically examined. Flavoring samples were extracted with 10 m L V（ n-hexane） ∶ V（ ethyl acetate） = 1∶ 1,for 30 min by ultrasonic extraction and cleaned up by florisil solid phase extraction cartridge,then detected by GC-TOFMS. Accurate mass analysis,chlorine isotopic peak clusters,fragment ion abundance ratios and retention time were employed to qualitative identification and internal standard method was used for quantitative determination. The results indicated that the linear correlation coefficients（ r2） were greater than 0. 998 6,the relative standard deviations（ RSD） were lower than 4. 5%,the limits of detection ranged from 0. 14 to 0. 21 μg / kg,and the recoveries of 3 pesticides ranged from 87% to 107%. This method is simple and rapid,with high accuracy and high sensitivity. It is appropriate for the rapidly screening and determination of pesticide residues in flavoring.

关 键 词：香精 农药 超声萃取 负化学电离源 飞行时间质谱 

分 类 号：O657.63[理学—分析化学] F767.2[理学—化学]