PDF《超高效液相色谱 ⁃串联质谱法快速测定鸡蛋中 氟虫腈及其代...》

2018 年8月Vol.

36 No.8 August

2018 Chinese Journal of Chromatography 745~751 研究论文 DOI: 10.3724/ SP.J.1123.2018.03012 ?收稿日期:2018?03?12 ?通讯联系人.Tel:(0574)89077438,E?mail:shufenzhang1128@ 163.com. 超高效液相色谱?串联质谱法快速测定鸡蛋中 氟虫腈及其代谢物残留 张爱芝, 李湘江, 王志强, 张书芬? , 宋悦, 曹丽丽, 蔡君美, 陈林吉 (宁波市食品检验检测研究院, 浙江 宁波 315048) 摘要:建立了超高效液相色谱?串联质谱(UPLC?MS/ MS)快速测定鸡蛋中氟虫腈及其代谢物的方法. 在2g鸡蛋中 加入

2 mL 水后,用4mL 乙腈提取,然后加入

1 g NaCl,于4℃以

9 000 r/ min 离心

10 min,稀释后过有机膜. 采用 C18 色谱柱(100 mm*2?

1 mm, 1?

7 μm)分离,在电喷雾电离源、负离子模式下进行多反应监测(MRM)采集. 结 果表明,氟虫腈及其代谢物在

3 个添加水平下的回收率为 77? 4% ~ 112? 1%,相对标准偏差为 4? 0% ~ 13? 6%,检出限 为0? 10~0?

43 μg/ kg. 该法简单、高效,可用于实际样品检测. 关键词:超高效液相色谱?串联质谱;

QuEChERS;

氟虫腈及其代谢物;

鸡蛋;

基质效应 中图分类号:O658 文献标识码:A 文章编号:1000?8713(2018)08?0745?07 Rapid determination of fipronil and its metabolite residues in eggs using ultra performance liquid chromatography? tandem mass spectrometry ZHANG Aizhi, LI Xiangjiang, WANG Zhiqiang, ZHANG Shufen? , SONG Yue, CAO Lili, CAI Juemei, CHEN Linji (Ningbo Institute for Food Control, Ningbo 315048, China) Abstract: A method was developed for the rapid simultaneous determination of fipronil and its metabolite residues in eggs using ultra performance liquid chromatography?tandem mass spec? trometry (UPLC?MS/ MS). The egg samples (2 g) with

2 mL water were extracted with

4 mL acetonitrile. After adding

1 g sodium chloride, the mixture was centrifuged at

9 000 r/ min for

10 min at

4 ℃. The suspension was diluted and filtered through a 0?

22 μm organic membrane. The analytes were separated on a C18 column (100 mm*2?

1 mm, 1?

7 μm), and detected under the multiple reaction monitoring (MRM) mode with a negative ESI source. The average recoveries of fipronil and its metabolites varied from 77? 4% to 112? 1%, and the relative standard devia? tions were between 4? 0% and 13? 6% at three spiked levels. The limits of detection ( LODs) ranged from 0?

10 μg / kg to 0?

43 μg / kg. The method is simple, effective, and can be applied to real samples. Key words: ultra performance liquid chromatography?tandem mass spectrometry (UPLC?MS/ MS);

QuEChERS;

fipronil and its metabolites;

eggs;

matrix effects

2017 年7月20 日,比利时通过欧盟食品饲料 类快速预警系统(RASFF)通报鸡蛋中检出氟虫腈, 截至

2017 年8月14 日,问题鸡蛋波及

20 个国家和 地区,被称为 毒鸡蛋 事件,引起公众广泛关注. 氟虫腈(fipronil)又名锐劲特(Regent),是一种苯基 吡唑类杀虫剂,对蚜虫、叶蝉、飞虱、鳞翅目幼虫、蝇 类和鞘翅目等一系列害虫均具有很高的杀虫活性. 研究表明,氟虫腈对蜜蜂及水产动物具有极高毒 色谱第36 卷性[1] ,国际食品法典委员会(CAC)[2] 和日本肯定列 表[3] 、美国相关标准[4] 、欧盟相关标准[5] 中规定氟 虫腈在蛋中的最大残留限量分别为 0?

02、0?

03 和0?

005 mg / kg. 我国于

2009 年10 月1日开始对该 农药限用,GB 2763?2016 中明确了氟虫腈及其代谢 物在谷物、油料、油脂、蔬菜、水果、糖类和食用菌中 的限量 ( 玉米及鲜食玉米为 0?