Simultaneous Determination of Residues of 14 Anesthetics in Freshwater Fish by Gas Chromatography-Triple Quadrupole Tandem Mass Spectrometry with Pass-Through Solid Phase Extraction
摘 要
提出了通过式固相萃取-气相色谱-三重四极杆串联质谱法(GC-MS/MS)同时测定淡水鱼中丁香酚、甲基丁香酚、异丁香酚、顺式-甲基异丁香酚、乙酸丁香酚酯、乙酰基异丁香酚、丙泊酚、三卡因、苯佐卡因、利多卡因、普鲁卡因、普莫卡因、丁卡因和布他卡因等14种麻醉剂残留量的方法。称取处理好的样品2 g,加入5.00 mg·L-1内标溶液100 μL和水5 mL,涡旋混匀,静置30 min。加入乙腈10 mL提取,再加入氯化钠2 g盐析分层,离心,取5 mL上清液加载到PRiME HLB柱上,收集流出液。取2 mL流出液,加入二甲基亚砜50 μL,常温下氮吹至近干,用丙酮1.0 mL复溶,经0.22 μm微孔滤膜过滤,滤液供GC-MS/MS测定。采用HP-5MS UI毛细管色谱柱分离各目标物,以电子轰击离子源和多反应监测模式检测,内标法定量。结果表明:14种麻醉剂工作曲线的线性范围为0.005~0.400 mg·L-1,检出限为0.001 mg·kg-1;以阴性样品为基质进行3个浓度水平的加标回收试验,日内、日间回收率为75.3%~120%,日内、日间精密度(n=6)为1.3%~10%;方法用于33份实际样品分析,有15份样品中检出丁香酚,检出量为0.013 6~0.462 mg·kg-1。
Abstract
A method for the determination of residues of 14 anesthetics, including eugenol, methyleugenol, isoeugenol, cis-methyl isoeugenol, eugenyl acetate, acetyl isoeugenol, propofol, tricaine, benzocaine, lidocaine, procaine, pramoxine, tetracaine and butacaine, in freshwater fish by gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS) with pass-through solid phase extraction was proposed. The processed sample (2 g) was taken, and 100 μL of 5.00 mg·L-1 internal standard solution and 5 mL of water were added. The mixture was mixed well by vortex, and settled for 30 min. Acetonitrile (10 mL) was added into above mixture for extraction, and 2 g of sodium chloride was added for salting out stratification. After centrifugation, 5 mL of the supernatant was loaded onto PRiME HLB column, and the effluent was collected. An aliquot (2 mL) was taken, and 50 μL of dimethyl sulfoxide was added. The solution was blown to nearly dryness at room temperature by nitrogen. Then the residue was redissolved with 1.0 mL of acetone, and filtered by 0.22 μm microporous membrane. The filtrate was determined by GC-MS/MS. HP-5MS UI capillary column was used to separate target compounds, and electron impact ion source and multiple reaction monitoring mode were used for detection, with internal standard method for quantification. It was shown that the linear ranges of working curves of 14 anesthetics were 0.005-0.400 mg·L-1, with the same detection limits of 0.001 mg·kg-1. Test for recovery was made on negative sample as matrix at 3 concentration levels by addition standard method, giving values of recovery of intra-day and inter-day were in the range of 75.3%-120%, and precision (n=6) of intra-day and inter-day were in the range of 1.3%-10%. This method was applied to the analysis of 33 actual samples, and eugenol was detected in 15 samples, with detection amounts in the range of 0.013 6-0.462 mg·kg-1.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202210003
所属栏目 试验与研究
基金项目
收稿日期 2022/2/14
修改稿日期
网络出版日期
作者单位点击查看
备注赵莹,博士,主要从事食品卫生理化检验
引用该论文: ZHAO Ying,YIN Danyang,WANG Wei,HU Jiawei. Simultaneous Determination of Residues of 14 Anesthetics in Freshwater Fish by Gas Chromatography-Triple Quadrupole Tandem Mass Spectrometry with Pass-Through Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2022, 58(10): 1130~1136
赵莹,尹丹阳,王玮,胡佳薇. 通过式固相萃取-气相色谱-三重四极杆串联质谱法同时测定淡水鱼中14种麻醉剂的残留量[J]. 理化检验-化学分册, 2022, 58(10): 1130~1136
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】金元,何雅静,程波,等.丁香酚类麻醉剂的安全性探讨[J].食品安全质量检测学报, 2017,8(1):33-40.
【2】黄艳婷,庄玥,邱蕴绮.高效液相色谱法快速测定外用成人用品中16种局麻成分[J].分析测试学报, 2020,39(12):1533-1537.
【3】王欢,胡磊,周明昊.固相萃取与液相色谱质谱联用技术测定化妆品中7种局部麻醉药[J].日用化学品科学, 2017,40(9):30-34.
【4】PRAMOD P K, RAMACHANDRAN A, SAJEEVAN T P, et al. Comparative efficacy of MS-222 and benzocaine as anaesthetics under simulated transport conditions of a tropical ornamental fish Puntius filamentosus (Valenciennes)[J]. Aquaculture Research, 2010,41(2):309-314.
【5】CARTER K M, WOODLEY C M, BROWN R S. A review of tricaine methanesulfonate for anesthesia of fish[J]. Reviews in Fish Biology and Fisheries, 2011,21(1):51-59.
【6】翟纹静,朱振华,王莉莉,等.用三重四极杆气质联用仪测定水产品中多种麻醉剂[J].大连海洋大学学报, 2018,33(6):769-774.
【7】滕雪,王国年.成人丙泊酚输注综合征研究进展[J].临床麻醉学杂志, 2016,32(4):402-403.
【8】颜珲璘,黄和,高平,等.高效液相色谱荧光法测定水产品中丙泊酚麻醉剂的残留量[J].分析试验室, 2019,38(8):955-958.
【9】王彩霞,熊光权,白婵,等.高效液相色谱法检测鮰鱼体内丁香酚的残留[J].食品安全质量检测学报, 2019,10(8):2195-2200.
【10】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.
【11】禤开智,梁振纲,陈文慧,等.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.
【12】吴少明,蔡小明,周鹏,等.超高效液相色谱-串联质谱法同时测定水产品中6种丁香酚类物质的残留量[J].食品科学, 2020,41(16):320-326.
【13】陈焕,黄和,高平,等.分散固相萃取-气相色谱法同时测定水产品中六种丁香酚类麻醉剂的残留量[J].食品工业科技, 2015,36(8):88-92.
【14】柯常亮,刘奇,陈洁文,等.气相色谱-串联质谱联用法测定水中丁香酚残留[J].中国渔业质量与标准, 2014,4(4):49-55.
【15】余颖.气相色谱-质谱法测定鱼肉中丁香酚的残留[J].福州大学学报(自然科学版), 2015,43(2):266-270.
【2】黄艳婷,庄玥,邱蕴绮.高效液相色谱法快速测定外用成人用品中16种局麻成分[J].分析测试学报, 2020,39(12):1533-1537.
【3】王欢,胡磊,周明昊.固相萃取与液相色谱质谱联用技术测定化妆品中7种局部麻醉药[J].日用化学品科学, 2017,40(9):30-34.
【4】PRAMOD P K, RAMACHANDRAN A, SAJEEVAN T P, et al. Comparative efficacy of MS-222 and benzocaine as anaesthetics under simulated transport conditions of a tropical ornamental fish Puntius filamentosus (Valenciennes)[J]. Aquaculture Research, 2010,41(2):309-314.
【5】CARTER K M, WOODLEY C M, BROWN R S. A review of tricaine methanesulfonate for anesthesia of fish[J]. Reviews in Fish Biology and Fisheries, 2011,21(1):51-59.
【6】翟纹静,朱振华,王莉莉,等.用三重四极杆气质联用仪测定水产品中多种麻醉剂[J].大连海洋大学学报, 2018,33(6):769-774.
【7】滕雪,王国年.成人丙泊酚输注综合征研究进展[J].临床麻醉学杂志, 2016,32(4):402-403.
【8】颜珲璘,黄和,高平,等.高效液相色谱荧光法测定水产品中丙泊酚麻醉剂的残留量[J].分析试验室, 2019,38(8):955-958.
【9】王彩霞,熊光权,白婵,等.高效液相色谱法检测鮰鱼体内丁香酚的残留[J].食品安全质量检测学报, 2019,10(8):2195-2200.
【10】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.
【11】禤开智,梁振纲,陈文慧,等.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.
【12】吴少明,蔡小明,周鹏,等.超高效液相色谱-串联质谱法同时测定水产品中6种丁香酚类物质的残留量[J].食品科学, 2020,41(16):320-326.
【13】陈焕,黄和,高平,等.分散固相萃取-气相色谱法同时测定水产品中六种丁香酚类麻醉剂的残留量[J].食品工业科技, 2015,36(8):88-92.
【14】柯常亮,刘奇,陈洁文,等.气相色谱-串联质谱联用法测定水中丁香酚残留[J].中国渔业质量与标准, 2014,4(4):49-55.
【15】余颖.气相色谱-质谱法测定鱼肉中丁香酚的残留[J].福州大学学报(自然科学版), 2015,43(2):266-270.
相关信息