|本期目录/Table of Contents|

[1]李宇翔,李燕平,李少光,等.UPLC-Q-Exactive测定茶叶中的氟虫腈及其代谢物[J].福建医科大学学报,2020,54(01):1-7.
 LI Yuxiang,LI Yanping,LI Shaoguang,et al.Determination of Fipronil and its Metabolites in Tea by UPLC-Quadrupole-Electrostatic Field/Orbitrap High Resolution Mass Spectrometry[J].Journal of Fujian Medical University,2020,54(01):1-7.
点击复制

UPLC-Q-Exactive测定茶叶中的氟虫腈及其代谢物(PDF)
分享到:

《福建医科大学学报》[ISSN:1672-4194/CN:35-1192/R]

卷:
第54卷
期数:
2020年01期
页码:
1-7
栏目:
论著
出版日期:
2020-02-28

文章信息/Info

Title:
Determination of Fipronil and its Metabolites in Tea by UPLC-Quadrupole-Electrostatic Field/Orbitrap High Resolution Mass Spectrometry
文章编号:
1672-4194(2020)01-0001-07
作者:
李宇翔1 李燕平2 李少光3 杨 艳1
1.福建省人兽共患病研究重点实验室,福建省疾病预防控制中心,福州 350001; 2.福建省产品质量检验研究院,福州 350001; 3.福建医科大学 药学院,福州 350122
Author(s):
LI Yuxiang1 LI Yanping2 LI Shaoguang3 YANG Yan1
1.Fujian Provincial Key Laboratory of Zoonosis Research, Fujian Center for Disease Control& Prevention, Fuzhou 350001, China; 2.Fujian Inspection and Research Institute for Product Quality, Fuzhou 350001, China; 3.Faculty of Pharmacy, Fujian Medical University, Fuzhou 350122, China
关键词:
质谱分析法 电磁场 腈类 茶叶
Keywords:
mass spectrometry electromagnetic fields nitriles fluorine folium camelliae
分类号:
R05; R446.1; R916.4
DOI:
-
文献标志码:
A
摘要:
目的 建立一种UPLC-四极杆-静电场/轨道阱质谱仪(UPLC-Q-Exactive)快速筛查茶叶中氟虫腈及其代谢物。 方法 将茶叶样品均质后,加乙腈超声提取,再加NaCl、无水Na2SO4除水,最后加N-丙基乙二胺(PSA)粉末、C18粉末以及Na2SO4去除杂质、净化样品。选用Thermo Syncronis C18柱(100 mm×2.1 mm,1.7 μm)色谱柱对待测物进行色谱分离,分别采用一级全扫(Full MS/t-SIM)及二级平行监测(PRM)扫描模式进行定量定性分析。 结果 氟虫腈及其代谢物在0.1~2.0 μg/L线性范围内线性良好,其平均回收率和相对偏差为90.2%~106.7%和2.035%~5.438%(Full MS/t-SIM),92.0%~103.2%和1.075%~5.930%(PRM)。 结论 本方法操作简便、快速、重现性好、稳定性好、灵敏度高,适用于高通量茶叶中氟虫腈及其代谢物的快速定性定量筛查。
Abstract:
Objective A UPLC-quadrupole-electrostatic field/orbitrap high-resolution mass spectrometry was developed for rapid screening of fipronil and its metabolites in tea. Methods After homogenizing the tea samples, ultrasonic extraction with acetonitrile was added, then sodium chloride and anhydrous sodium sulfate were added to remove water. Finally, PSA powder, C18 powder and anhydrous sodium sulfate were added to remove impurities and purify the samples. Thermo Syncronis C18 column(100 mm×2.1 mm, 1.7 μm)was used for chromatographic separation of the samples. Data were collected under the Full MS/t-SIM and PRM scanning mode of Q-Exactive for qualitative and quantitative analysis. Results The linearity of Fipronil and its metabolites was good in the concentration range of 0.1-2.0 μg/L. The average recovery and RSD of the two scanning modes were 90.2%-106.7% and 2.035%-5.438%(Full MS/t-SIM), 92.0%-103.2% and 1.075%-5.930%(PRM). Conclusion The method is simple, rapid, reproducible, stable and sensitive. It is suitable for rapid qualitative and quantitative screening of Fipronil and its metabolites in tea.

参考文献/References:

[1] 童小麟,陈建民.出口茶叶中氟虫腈的残留现状分析与控制措施研究[J].检验检疫学刊,2013,23(4):72-76.
[2] 宁 霄,金绍明,高文超,等.QuEChERS-超高效液相色谱-串联质谱法测定动物源性食品中氟虫腈及其代谢物残留[J].分析化学,2018,46(8):1297-1305.
[3] 白宝清,李美萍,张生万.QuEChERS-DLLME-高效液相色谱法测定蔬菜中溴虫腈和氟虫腈残留[J]. 食品科学,2014,35(24):254-258.
[3] 田 丽,王彩霞,胡佳薇,等.气相色谱-电子捕获法和气相色谱-质谱法测定水果中氟虫腈残留[J].中国卫生检验杂志,2016,26(14):1997-1999.
[4] 周 昱,徐敦明,陈达捷,等.固相微萃取-气相色谱法和气相色谱-质谱法测定茶叶中氟虫腈及其代谢物残留[J].色谱,2011,29(7):656-664.
[5] 叶 倩,邓义才,路大海,等.气相色谱法测定蔬菜水果中氟虫腈等6种农药残留[J].农药,2016,55(1):51-54.
[6] 叶 倩,邓义才,梁应坤,等.气相色谱-质谱法(GC-MS)测定蔬菜水果中氟虫腈及其代谢物残留[J].农药,2017,56(3):203-206.
[7] 胡贵祥,夏 祥,朱惠芳.QuEChERS在线凝胶色谱-气相色谱/质谱联用法测定水果蔬菜中氟虫腈农药残留[J].化学试剂,2017,39(5):509-512.
[8] 张云升,李志伟.高效液相色谱法测定氟虫腈[J].河北省科学院学报,2010,27(2):40-42.
[9] 林 涛,樊建麟,杨东顺,等.低温液液萃取/超高效液相色谱-串联质谱法快速测定鲜枣中氟虫腈及代谢物[J].分析测试学报,2015,34(12):1360-1365.
[10] 邬 阳,郭 艳,郭艳琼,等.高效液相色谱-质谱法测定果蔬中氟虫腈等7种农药残留的方法研究[J].北方农业学报,2017,45(1):70-75.
[11] Ramasubramanian T,Paramasivam M,Jayanthi R,et al.A simple and sensitive single-step method for gas chromatography-mass spectrometric determination of fipronil and its metabolites in sugarcane juice, jaggery and sugar[J].Food Chemistry,2014,150:408-413.
[12] 董亚蕾,刘文婧,曹 进,等.QuEChERS-超高效液相色谱-串联质谱法测定坚果中38种农药残留[J].分析化学,2017, 45(9):1397-1404.
[13] 吕 冰,尹帅星,陈达炜,等.QuEChERS-四极杆/静电场轨道阱高分辨质谱测定动物性食品中氟虫腈及其代谢物残留[J].分析测试学报,2017,36(12):1424-1430.
[14] 严 凤,李丹妮,吴剑平,等.超高效液相色谱-四级杆/静电场轨道阱高分辨质谱筛查测定饲料中19种磺胺类药物[J].中国兽药杂志,2016,50(2):29-36.
[15] 孙碧霞,郭德华,丁卓平,等.离子阱-飞行时间串联质谱快速筛查蔬菜中189种农药残留[J].分析测试学报,2010,29(10):1017-1024.
[16] Fedorova G,Randak T,Lindberg R H, et al.Comparison of the quantitative performance of a Q-Exactive high-resolution mass spectrometer with that of a triple quadrupole tandem mass spectrometer for the analysis of illicit drugs in wastewater[J].Rapid Communications in Mass Spectrometry,2013,27(15):1751-1762.

相似文献/References:

备注/Memo

备注/Memo:
收稿日期: 2019-04-01 基金项目: 福建省卫计委青年课题(2015-1-21,2016-02-10) 作者简介: 李宇翔,男,主管技师,医学硕士 通讯作者: 杨 艳. Email: 229638337@qq.com
更新日期/Last Update: 2020-01-30