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超高效液相色谱-串联质谱法同时检测鱼肉中5种渔用麻醉剂残留
其他题名Determination of 5 kinds of fish anesthetics residues in fish by ultra-high performance liquid chromatography-tandem mass spectrometry
刘平1; 辛爽英2; 范赛1; 王莉莉1; 罗仁才1; 吴国华1; 赵榕1; 赵耀1
来源期刊卫生研究
ISSN1000-8020
出版年2019
卷号48期号:4页码:640-645,650
中文摘要目的建立超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定鱼肉中丁香酚、甲基丁香酚、甲基异丁香酚、乙酰基异丁香酚及3-氨基苯甲酸乙酯甲基磺酸盐(MS-222)残留量的方法。方法匀浆后的鱼肉经乙腈-水(80 ∶20,V/V)提取,经 Oasis PRiME HLB固相萃取小柱净化,离心浓缩后,Waters ACQUITY UPLC BEH Phenyl柱(2.1 mm*100 mm,1.7 mum)分离,采用三重四级杆质谱的多反应监测模式进行测定。结果5种渔用麻醉剂在各自浓度范围内线性关系良好(r~2>0.995),以空白鱼肉为基质进行3个水平加标回收实验,回收率为72.6%~106.0%,相对标准偏差为2.2%~20.1%(n=6),方法检出限为0.14 ~0.30 mug/kg,定量限为0.5 ~1.0 mug/kg。结论该法操作简便,快速可靠,成功实现了甲基丁香酚和甲基异丁香酚同分异构体的分离,可节约大量有机溶剂,适合大量鱼肉样品中5种渔用麻醉剂的筛选和检测。
英文摘要OBJECTIVE A method for the simultaneous determination of 5 kinds of fish anesthetics residues in fish has been developed by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).Eugenol,methyleugenol,methyl-isoeugenol,acetyl-isoeugenol and tricaine methanesulfonate (MS-222) were concerned.METHODS After homogenization fish samples were extracted by acetonitrile-water (80 ∶ 20,V/V),purified by Oasis PRiME HLB solid-phase extraction column.Then after centrifuged and concentrated,the samples were separated by Waters ACQUITY UPLC BEH Phenyl column(2.1 mm*100 mm,1.7 mum).The detection was confirmed and quantified by mass spectrum of triple quadrupole in the multiple reaction monitoring (MRM) mode.RESULTS The calibration curves showed good linearity in each range with correlation coefficients greater than 0.995.Three levels spiked recovery experiments were carried out using blank fish mud extraction as substrate,the recoveries ranged from 72.6% to 106.0%,the relative standard deviations (RSDs) ranged from 2.2% to 20.1%(n=6).The qualitative limits of detections (S/N>3) were 0.14-0.30 mug/kg and the quantitative limits(S/N>10) were 0.5-1.0 mug/kg.CONSLUSION The method is simple and easy to operate,with less organic reagent,high sensitivity and good stability.The isomers of methyl eugenol and methyl isoeugenol were successfully separated.It is suitable for the detection of 5 kinds of fish anesthetics in fish.
中文关键词渔用麻醉剂 ; 丁香酚 ; 3-氨基苯甲酸乙酯甲基磺酸盐(MS-222) ; 超高效液相色谱-串联质谱 ; 食品检测
英文关键词fish anesthetic eugenol tricaine methanesulfonate (MS-222) UPLC-MS/MS food detection
语种中文
国家中国
收录类别CSCD
WOS类目PUBLIC ENVIRONMENTAL OCCUPATIONAL HEALTH
WOS研究方向Public, Environmental & Occupational Health
CSCD记录号CSCD:6545500
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/239591
作者单位1.北京市疾病预防控制中心北京市预防医学研究中心, 北京 100013, 中国;
2.辛集市市场监督管理局, 辛集, 052360
推荐引用方式
GB/T 7714
刘平,辛爽英,范赛,等. 超高效液相色谱-串联质谱法同时检测鱼肉中5种渔用麻醉剂残留[J],2019,48(4):640-645,650.
APA 刘平.,辛爽英.,范赛.,王莉莉.,罗仁才.,...&赵耀.(2019).超高效液相色谱-串联质谱法同时检测鱼肉中5种渔用麻醉剂残留.卫生研究,48(4),640-645,650.
MLA 刘平,et al."超高效液相色谱-串联质谱法同时检测鱼肉中5种渔用麻醉剂残留".卫生研究 48.4(2019):640-645,650.
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