Please wait a minute...
 
 
食品与发酵工业  2021, Vol. 47 Issue (13): 280-285    DOI: 10.13995/j.cnki.11-1802/ts.026943
  分析与检测 本期目录 | 过刊浏览 | 高级检索 |
高效液相色谱-串联质谱法测定动物源性食品中噻节因残留
肖泳*, 周丛, 邓航, 冯燕英, 潘照, 唐吉旺, 袁列江
(湖南省产商品质量监督检验研究院,湖南 长沙,410007)
Determination of dimethipin residues in animal derived food by HPLC-MS/MS
XIAO Yong*, ZHOU Cong, DENG Hang, FENG Yanying, PAN Zhao, TANG Jiwang, YUAN Liejiang
(Hunan Province Produce Commodity Quality Supervision Testing & Research Institute,Changsha 410007,China)
下载:  HTML  PDF (1730KB) 
输出:  BibTeX | EndNote (RIS)      
摘要 建立了高效液相色谱-串联质谱测定动物源性食品中噻节因残留的分析方法。样品经体积分数1%的乙酸乙腈溶液提取、正己烷脱脂、C18固相萃取柱净化,采用Venusil MP C18(2)色谱柱(150 mm×2.1 mm,3 μm)分离,以乙腈和水为流动相进行梯度洗脱,采用大气压化学电离源电离、负离子模式扫描,多反应监测模式检测,内标法定量。结果表明:噻节因质量浓度在1.0~500.0 μg/L范围内呈良好线性,相关系数(R2)为0.999 3,方法的定量限为1.0 μg/kg;以猪肉、猪肝、牛肉、牛肝、羊肉、羊肝、鸡肉、鸡胗、鸡蛋和牛奶为基质,噻节因在1.0、10.0和100.0 μg/kg 3个水平下的平均加标回收率为89.0%~105.0%,相对标准偏差为2.20%~7.64%。该方法基质干扰小、灵敏度高、准确可靠、适用于动物源性食品中噻节因残留的定量检测。
服务
把本文推荐给朋友
加入引用管理器
E-mail Alert
RSS
作者相关文章
肖泳
周丛
邓航
冯燕英
潘照
唐吉旺
袁列江
关键词:  高效液相色谱-串联质谱  固相萃取  噻节因  动物源性食品    
Abstract: A method for the determination of dimethipin residues in animal derived food by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed. The samples were extracted with acetonitrile containing 1% (V/V) acetic acid and defatted with n-hexane, followed by clean-up using C18 solid phase extraction column. The analytes were separated on a Venusil MP C18 (2) column (150 mm×2.1 mm, 3 μm) under a gradient elution program using acetonitrile and water was used as the mobile phases. The analytes were detected by tandem mass spectrometry using a negative atmospheric pressure chemical ionization (APCI-) source in the multiple reaction monitoring (MRM) mode. The internal standard calibration curves were used for quantitative analysis. The results showed that calibration curves had good linearities in the range of 1.0-500.0 μg/L for dimethipin, which with a correlation coefficients (R2) 0.999 3. The limit of quantification (LOQ) of the method was 1.0 μg/kg. The average recoveries of dimethipin in pork, pig liver, beef, beef liver, mutton, sheep liver, chicken, chicken gizzard, egg and milk matrices at spiked levels of 1.0, 10.0 and 100.0 μg/kg were 89.0%-105.0%, and the relative standard deviations were 2.20%-7.64%. The method has less matrix interference, with high sensitivity, accuracy and reliability, and it is suitable for the quantitative detection of dimethipin residues in animal derived food.
Key words:  high performance liquid chromatography-tandem mass spectrometry    solid phase extraction    dimethipin    animal derived foods
收稿日期:  2021-02-07      修回日期:  2021-03-09           出版日期:  2021-07-15      发布日期:  2021-08-02      期的出版日期:  2021-07-15
基金资助: 湖南省市场监督管理局科技计划项目(2020KJJH13)
作者简介:  硕士,工程师(通讯作者,E-mail:xy882008@163.com)
引用本文:    
肖泳,周丛,邓航,等. 高效液相色谱-串联质谱法测定动物源性食品中噻节因残留[J]. 食品与发酵工业, 2021, 47(13): 280-285.
XIAO Yong,ZHOU Cong,DENG Hang,et al. Determination of dimethipin residues in animal derived food by HPLC-MS/MS[J]. Food and Fermentation Industries, 2021, 47(13): 280-285.
链接本文:  
http://sf1970.cnif.cn/CN/10.13995/j.cnki.11-1802/ts.026943  或          http://sf1970.cnif.cn/CN/Y2021/V47/I13/280
[1] POTTER T L,MARTI L,BELFLOWER S,et al.Multiresidue analysis of cotton defoliant,herbicide,and insecticide residues in water by solid-phase extraction and GC-NPD,GC-MS,and HPLC-diode array detection[J].Journal of Agricultural and Food Chemistry,2000,48(9):4 103-4 108.
[2] 孙武勇, 魏东伟,刘海芳,等.高效液相色谱法测定棉花中3种脱叶剂的残留量[J].理化检验(化学分册),2014,50(1):112-113.SUN W Y,WEI D W,LIU H F,et al.Determination of three defoliant residues in cotton by high performance liquid chromatography[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis),2014,50(1):112-113.
[3] KIM Y J,CHOI Y H,SHIN B W,et al.Comparison between the liquid-liquid partition method and modified QuEChERS method for the analysis of pesticide residues in beef fat[J].Korean Journal of Veterinary Service,2011,34(4):429-439.
[4] 李凯, 刘永强,张金玲,等.DPX-Q萃取吸管结合气相色谱/串联质谱法同时检测水果蔬菜中102种农药残留[J].分析试验室,2015,34(2):236-242.LI K,LIU Y Q,ZHANG J L,et al.Application of DPX-Q tips for analysis of 102 pesticide residues in fruits and vegetables by GC-MS[J].Chinese Journal of Analysis Laboratory,2015,34(2):236-242.
[5] 吴卫东, 洪小柳,孙娅楠,等.GC-MS/MS快速检测香港《食物内除害剂残余规例》中的101种除害剂残留量[J].环境化学,2016,35(10):2 215-2 220.WU W D,HONG X L,SUN Y N,et al.Rapid determination of 101 pesticide residues of HongKong regulation by GC-MS/MS[J].Environmental Chemistry,2016,35(10):2 215-2 220.
[6] 张权, 沙比拉·吐拉江,周贻兵,等.不同种类固相萃取柱测定韭菜中58种农药残留量的净化效果比较[J].食品工业科技,2019,40(20):243-250;261.ZHANG Q,SHABILA T L J,ZHOU Y B,et al.Comparison of purfication effect of different types of SPE column on the dertermination of 58 pesticide residues in chives[J].Science and Technology of Food Industry,2019,40(20):243-250;261.
[7] 李南, 石志红,庞国芳,等.坚果中185种农药残留的气相色谱-串联质谱法测定[J].分析测试学报,2011,30(5):513-521.LI N,SHI Z H,PANG G F,et al.Determination of 185 pesticide residues in nuts by gas chromatography tandem mass spectrometry[J].Journal of Instrumental Analysis,2011,30(5):513-521.
[8] 史晓梅, 章晴,杨永坛,等.凝胶渗透色谱净化结合气相色谱-三重四极杆质谱法测定植物油中多农药残留量[J].中国粮油学报,2017,32(10):156-162.SHI X M,ZHANG Q,YANG Y T,et al.Determination of multi-pesticides residues in vegetable oil by gel permeation chromatography purifying method combined with gas chromatography tandem mass spectrometry[J].Journal of the Chinese Cereals and Oils Association,2017,32(10):156-162.
[9] 黄宗兰, 陈沙,朱作为,等.气相色谱-三重四级杆串联质谱法同时测定西红柿中47种农药残留[J].食品安全质量检测学报,2018,9(5):1 142-1 148.HUANG Z L,CHEN S,ZHU Z W,et al.Simultaneous determination of 47 pesticide residues in tomato by gas chromatography-triple quadrupole mass spectrometry[J].Journal of Food Safety and Quality,2018,9(5):1 142-1 148.
[10] 张煜卓, 于湛,李硕,等.应用QuEChERS技术与气相色谱-串联质谱法同时检测南果梨中16种农药残留[J].现代预防医学,2019,46(2):327-331.ZHANG Y Z,YU Z,LI S,et al.Simultaneous determination of 16 pesticide residues in Nanguo pear by QuEChERS combined with gas chromatography-tandem mass spectrometry[J].Modern Preventive Medicine,2019,46(2):327-331.
[11] 马驰远, 段吴燕,罗秋红,等.GC-MS/MS法与HPLC-MS/MS法相结合检测果蔬中农药多残留[J].江西化工,2019(1):119-128.MA C Y,DUAN W Y,LUO Q H,et al.Determination of pesticide residues in fruits and vegetables by GC-MS/MS combined with HPLC-MS/MS[J].Jiangxi Chemical Industry,2019(1):119-128.
[12] 杨涛, 王静静,鹿毅.HPLC-APCI-MS/MS检测果蔬中噻节因残留的方法研究[J].广州化工,2013,41(8):126-128.YANG T,WANG J J,LU Y.Study on the method of detection dimethipin residues in fruits and vegetables by HPLC-APCI-MS/MS[J].Guangzhou Chemical Industry,2013,41(8):126-128.
[13] 田海, 冯玉洁,张艳玲,等.超高效液相色谱串联质谱法测定鸡肉中噻节因残留[J].现代农药,2017,16(4):39-41.TIAN H,FENG Y J,ZHANG Y L,et al.Determination of dimethipin residues in chicken by ultra-high performance liquid chromatography-tandem mass spectrometry[J].Modern Agrochemicals,2017,16(4):39-41.
[14] 田海, 冯玉洁,郇志博,等.超高效液相色谱串联质谱法测定鸡蛋中噻节因残留[J].中国科技成果,2019,20(5):32-34.TIAN H,FENG Y J,XUN Z B,et al.Determination of dimethipin residues in egg by ultra-high performance liquid chromatography-tandem mass spectrometry[J].China Science and Technology Achievements,2019,20(5):32-34.
[15] MATUSZEWSKI B K,CONSTANZER M L,CHAVEZ-ENG C M.Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS[J].Analytical Chemistry,2003,75(13):3 019-3 030.
[1] 范金平, 张盈, 魏进, 罗世霞, 段婷婷. QuEChERS结合超高效液相色谱串联质谱法测定花椒中烯效唑残留量及贮藏稳定性[J]. 食品与发酵工业, 2021, 47(8): 230-235.
[2] 钟冬莲, 莫润宏, 王蕤, 喻宁华, 沈丹玉, 汤富彬. 反相聚合物固相萃取-气相色谱-质谱法测定植物油中角鲨烯和四种植物甾醇[J]. 食品与发酵工业, 2021, 47(4): 231-236.
[3] 廖若宇, 张春娥, 刘新保, 孙悦, 田建文. 黑米中合成着色剂亮蓝的提取工艺优化及含量测定[J]. 食品与发酵工业, 2021, 47(3): 120-127.
[4] 张洋, 李晓娟, 汪春明, 施鹏斐, 李淑娟. 离线固相萃取-气相色谱法定量分析巧克力中饱和烃类矿物油[J]. 食品与发酵工业, 2021, 47(21): 253-258.
[5] 李红丽, 吴晓琴, 赵博, 候美玲, 吴彦蕾, 黄先亮. QuEChERS-UPLC-MS/MS同时测定动物性食品中24种残留兽药的基质效应[J]. 食品与发酵工业, 2021, 47(20): 253-259.
[6] 黄永桥, 杨昌彪, 马凯, 毛敏霞, 简银池. QuEChERS结合UHPLC-MS/MS法测定畜肉中阿苯达唑及其代谢物的残留量[J]. 食品与发酵工业, 2021, 47(19): 258-263.
[7] 范清涛, 邓建朝, 张宾, 陈胜军, 杨贤庆, 李春生, 潘创, 王迪. 养殖虾类中呋喃西林代谢物检测方法的优化[J]. 食品与发酵工业, 2021, 47(16): 233-238.
[8] 李林竹, 马凯, 杨昌彪, 黄永桥, 王媛媛, 范金旭, 陶光灿. QuEChERS-超高效液相色谱-串联质谱法检测腌腊肉中四种常用香料[J]. 食品与发酵工业, 2021, 47(16): 247-252.
[9] 罗任杰, 林勤保, 颜建伟, 马俊杰, 李忠. PET/PE复合膜中初级芳香胺及2种塑料添加剂的迁移研究及安全评估[J]. 食品与发酵工业, 2021, 47(15): 120-128.
[10] 刘桂亮, 廉贞霞, 公丕学, 薛霞, 刘艳明, 祝建华. 固相萃取-高效液相色谱法测定食品中二氢槲皮素[J]. 食品与发酵工业, 2021, 47(15): 280-285.
[11] 李志霞, 董超, 周杰, 安文进, 张耀海, 李晶, 王成秋, 梁国鲁, 焦必宁. 柑橘中高风险农药及主要代谢物的消解转化特征及健康风险评价[J]. 食品与发酵工业, 2021, 47(14): 45-50.
[12] 薛霞, 赵慧男, 魏莉莉, 丁一, 宿书芳, 卢兰香, 王骏, 刘艳明, 胡梅. 超高效液相色谱-串联质谱法测定蜂蜜中五种水溶性维生素的含量[J]. 食品与发酵工业, 2021, 47(12): 250-256.
[13] 刘镇, 张瑛, 郑云峰, 胡翎榆, 屠生辉, 吴坚. 离子交换固相萃取-反相高效液相色谱法测定黄酒中游离嘌呤[J]. 食品与发酵工业, 2021, 47(11): 236-240.
[14] 田金凤, 尚远宏. QuEChERS净化-超高效液相色谱-串联质谱法测定凯特芒果中14种农药残留[J]. 食品与发酵工业, 2020, 46(9): 272-277.
[15] 叶佳明, 王京, 叶磊海, 何斌, 仰海青, 汪庆旗, 陈青俊. 在线固相萃取-二维色谱快速测定配方奶粉、米粉中维生素D的含量[J]. 食品与发酵工业, 2020, 46(7): 239-243.
No Suggested Reading articles found!
Viewed
Full text


Abstract

Cited

  Shared   
  Discussed   
版权所有 © 《食品与发酵工业》编辑部
地址:北京朝阳区酒仙桥中路24号院6号楼111室
本系统由北京玛格泰克科技发展有限公司设计开发  技术支持:support@magtech.com.cn