Simutanous Determination of 5 Anesthetic Residues in Fish by High Performance Liquid Chromatography-Tandem Mass Spectrometry with QuEChERS Extration
摘 要
建立了同时测定鱼肉中5种麻醉剂(苯佐卡因、利多卡因、普鲁卡因、普莫卡因、丁卡因)残留量的QuEChERS提取-高效液相色谱-串联质谱法。称取试样5.000 g,加入10 mL乙腈和QuEChERS提取试剂包(含4 g MgSO4和1 g NaCl),涡旋振荡5 min,以9 000 r·min-1转速离心4 min,吸取上层提取液5 mL,加入QuEChERS净化试剂包(含150 mg N-丙基乙二胺和150 mg C18),涡旋振荡3 min,以9 000 r·min-1转速离心4 min,取部分上清液过0.22 μm有机滤膜,移取200 μL滤液和800 μL 0.1%(体积分数,下同)甲酸溶液混合。以Thermo RP-MS色谱柱(150 mm×3 mm,2.6 μm)为固定相,乙腈-0.1%甲酸溶液为流动相进行梯度洗脱,质谱分析中选择电喷雾正离子源和多反应监测模式。采用基质匹配标准溶液消除基质效应,以外标法定量。5种麻醉剂的质量浓度在5.0~100 μg·L-1内对应的峰面积呈线性关系,检出限(3S/N)为0.05~0.3 μg·kg-1。加标回收率为71.0%~102%,测定值的相对标准偏差(n=6)为1.8%~9.8%。
Abstract
A method of high performance liquid chromatography-tandem mass spectrometry combined with QuEChERS extraction was developed for the simultaneous determination of 5 anesthetic residues, including benzocaine, lidocaine, procaine, pramocaine and tetracainein, in fish. 10 mL of acetonitrile and QuEChERS extraction reagent package (containing 4 g of MgSO4 and 1 g of NaCl) were added to 5.000 g of sample, and the mixture was vortexed for 5 min, then centrifuged at 9 000 r·min-1 for 4 min. 5 mL of the upper extract was added to QuEChERS purification reagent package (containing 150 mg of PSA and 150 mg of C18), and the mixture was vortexed for 3 min, then centrifuged at 9 000 r·min-1 for 4 min. A portion of the supernatant was taken and filtrated through a 0.22 μm organic filter, and 200 μL of the filtrate was mixted with 800 μL of 0.1% (φ) formic acid solution. A Thermo RP-MS column (150 mm×3 mm, 2.6 μm) was used as the stationary phase, and the mixture of acetonitrile and 0.1% formic acid solution was used as the mobile phase for gradient elution. Electrospray positive ion source and multi-reaction monitoring mode were selected for mass spectrometry analysis. Matrix effect was eliminated using matrix-matched standard solutions and external standard method was used for quantification. Linear relationships were found between peak areas and mass concentration of the 5 anesthetics in the same range of 5.0-100 μg·L-1, and the detection limits (3S/N) were 0.05-0.3 μg·kg-1. Values of recovery obtained by standard addition method were in the range of 71.0%-102%, and RSDs (n=6) were in the range of 1.8%-9.8%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201812008
所属栏目 工作简报
基金项目 海南省自然科学基金(20153160)
收稿日期 2018/2/14
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备注禤开智,工程师,硕士,主要从事食品中有害物质检测工作,xkz711@163.com
引用该论文: XUAN Kaizhi,LIANG Zhengang,CHEN Wenhui,CHEN Yiwei. Simutanous Determination of 5 Anesthetic Residues in Fish by High Performance Liquid Chromatography-Tandem Mass Spectrometry with QuEChERS Extration[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(12): 1405~1409
禤开智,梁振纲,陈文慧,陈艺玮. QuEChERS提取-高效液相色谱-串联质谱法同时测定鱼肉中5种麻醉剂的残留量[J]. 理化检验-化学分册, 2018, 54(12): 1405~1409
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参考文献
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【4】李小兵,周兴华,陈鹏飞,等.活鱼运输中常见麻醉剂的使用方法[J].重庆水产, 2011(4):39-43.
【5】SIVERTSVIK M, JEKSRUD W K, ROSNES J T. A review of modified atmosphere packaging of fish and fishery products-Significance of microbial growth, activities and safety[J]. International Journal of food Science & Technology, 2010,37(2):107-127.
【6】ZAHL I H, KIESSLING A, SAMUELSEN O B, et al. Anesthesia induces strees in Athantic salmon(Salmo salar), Athantic cod(Gadus morhua) and Atlantic halibut(Hippoglossus hippoglossus)[J]. Fish Physiology and Biochemistry, 2010,36(3):719-730.
【7】李亚菲.浅析麻醉剂在水产品中的研究现状及措施[J].陕西农业科学, 2015,61(12):66-67.
【8】SOTO C G, BURHANUDDIN. Clove oil as a fish anaesthetic for measuring length and weight of rabbitfish (Siganus lineatus)[J]. Aquaculture, 1995,136(1/2):149-152.
【9】刘春花,赵长臣,巩华,等.丁香油麻醉剂在水产养殖上的应用研究进展[J].广东饲料, 2016,25(11):33-36.
【10】刘翠,吐尔洪·买买提,穆赫塔尔·伊米尔艾山.盐酸利多卡因分析方法进展[J].药物分析杂志, 2011(1):204-209.
【11】CAPRIOTTI A L, CAVALIERE C, GIANSANTI P, et al. Recent developments in matrix solid-phase dispersion extraction[J]. Journal of Chromatography A, 2010,1217(16):2521-2532.
【12】崔冶建,付亚平,施群,等.反相高效液相色谱法测定鱼脑中MS-222的浓度[J].中南民族大学学报(自然科学版), 1996(3):65-68.
【13】陈焕,黄和,高平,等.高效液相色谱法测定水产品中丁香酚类麻醉剂的残留量[J].食品与发酵工业, 2014,40(12):156-160.
【14】高平,黄和,刘文侠,等.固相萃取-高效液相色谱-荧光检测法测定水产品中4种丁香酚类化合物[J].中国食品卫生杂志, 2016,28(1):56-61.
【15】李晓晶,于鸿,彭荣飞,等.QuEChERS-超高效液相色谱-串联质谱法同时快速测定肉类食品中多种抗生素残留[J].中国食品卫生杂志, 2016,28(6):747-752.
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