GC-MS/MS Determination of Melamine in Poultry Eggs with Dispersive Solid Phase Extraction with Syringe
摘 要
采用注射式分散固相萃取-气相色谱-串联质谱法测定禽蛋中三聚氰胺的含量。禽蛋样品用乙腈提取后,加入无水硫酸镁和氯化钠,离心后,上清液用正己烷除脂。以丙基乙二胺和石墨化炭黑为分散固相吸附剂,进行注射式分散固相萃取,过滤后,滤液用氮气吹干后再进行衍生化。在气相色谱分离中采用DB-5MS石英毛细管色谱柱,在质谱分析中采用定时选择性反应监测模式。三聚氰胺的质量浓度在5.0~200.0 μg·L-1内与其对应的峰面积呈线性关系,测定下限(10S/N)为2.4~3.5 μg·L-1。以空白样品为基体进行加标回收试验,所得回收率为80.3%~103%,测定值的相对标准偏差(n=6)为0.60%~8.9%。
Abstract
GC-MS/MS was applied to the determination of melamine in poultry eggs with dispersive solid phase extraction with syringe. The poultry egg sample was extracted with acetonitrile, and then anhydrous magnesium sulfate and sodium chloride were added. After centrifugation, fat in the supernatant was removed with n-hexane. Dispersive solid phase extraction with syringe was adopted with PSA and GCB as dispersive solid phase adsorbent. After filtration, the filtrate was dried by nitrogen blowing and then derivatized. The DB-5MS quartz capillary chromatographic column was used for GC separation and the timed-selected reaction monitoring mode was adopted in MS determination. Linear relationship between values of peak area and mass concentration of melamine was kept in the range of 5.0-200.0 μg·L-1, with lower limits of determination (10S/N) in the range of 2.4-3.5 μg·L-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 80.3%-103%, with RSDs (n=6) in the range of 0.60%-8.9%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201811009
所属栏目 工作简报
基金项目 科技部项目(2017YFC1602001);重庆市基本科研业务(2013cstc-jbky-00569);重庆市科研院所绩效激励引导专项(cstc2017jxjl0083)
收稿日期 2018/1/2
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联系人作者柴勇(40080977@qq.com)
备注褚能明,助理研究员,硕士,研究方向为农产品质量安全
引用该论文: CHU Nengming,SHU Xiao,ZHANG Xuemei,LI Dianyan,MENG Xia,YANG Junying,CHAI Yong. GC-MS/MS Determination of Melamine in Poultry Eggs with Dispersive Solid Phase Extraction with Syringe[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(11): 1276~1280
褚能明,舒晓,张雪梅,李典晏,孟霞,杨俊英,柴勇. 注射式分散固相萃取-气相色谱-串联质谱法测定禽蛋中三聚氰胺[J]. 理化检验-化学分册, 2018, 54(11): 1276~1280
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参考文献
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【2】段文仲,马育松,陈瑞春,等.食品中三聚氰胺污染途径及控制对策研究[J].食品科学, 2010,31(1):283-286.
【3】王辉,董元华,安琼.环丙氨嗪(Cyromazine)的生物毒性与环境行为研究进展[J].农业工程学报, 2008,24(1):246-249.
【4】林祥梅,王建峰,贾广乐,等.三聚氰胺的毒性研究[J].毒理学杂志, 2008(3):216-218.
【5】张国文,汪佳蓉,杨佳.三聚氰胺对DNA潜在损伤作用的研究[J].分析试验室, 2010,29(2):10-13.
【6】黄华斌,庄峙厦,赵丽,等.分子印迹固相萃取技术-高效液相色谱法测定奶制品和饲料中三聚氰胺含量[J].理化检验-化学分册, 2014,50(10):1286-1290.
【7】XU Y, CHEN L, WANG H, et al. Preparation of magnetic strong cation exchange resin for the extraction of melamine from egg samples followed by liquid chromatography-tandem mass spectrometry[J]. Analytica Chimica Acta, 2010,661:35-41.
【8】XIA X, DING S, LI X, et al. Validation of a confirmatory method for the determination of melamine in egg by gas chromatography-mass spectrometry and ultra-performance liquid chromatography-tandem mass spectrometry[J]. Analytica Chimica Acta, 2009,651:196-200.
【9】赵永彪,李自春,刘婷,等.高效液相色谱法测定宠物食品中的三聚氰胺[J].分析试验室, 2008,27(增刊1):190-192.
【10】吴惠勤,黄芳,林晓珊,等.气相色谱-质谱法测定奶粉及奶制品中的三聚氰胺[J].分析测试学报, 2008,27(10):1044-1048.
【11】WANG P C, LEE R J, CHEN C Y, et al. Determination of cyromazine and melamine in chicken eggs using quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction coupled with liquid chromatography-tandem mass spectrometry[J]. Analytica Chimica Acta, 2012,752:78-86.
【12】GB/T 22388-2008原料乳与乳制品中三聚氰胺检测方法[S].
【13】ANASTASSIADES M, LEHOTAY S J, ŠTAJNBAHER D, et al. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and "dispersive solid-phase extraction" for the determination of pesticide residues in produce[J]. Journal of AOAC International, 2003,86(2):412-431.
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