UPLC-MS/MS法测定新疆冷水鱼中孔雀石绿与隐色孔雀石绿

doi:10.6048/j.issn.1001-4330.2019.07.016

新疆农业科学 ›› 2019, Vol. 56 ›› Issue (7): 1325-1332.DOI: 10.6048/j.issn.1001-4330.2019.07.016

• 土壤肥料·贮藏加工·植物保护·畜牧水产 • 上一篇下一篇

UPLC-MS/MS法测定新疆冷水鱼中孔雀石绿与隐色孔雀石绿

李晓岩¹, 武运², 王犁烨², 苏敏¹, 沈慧慧¹, 巴哈提古丽·马那提拜¹

1.新疆出入境检验检疫局技术中心,乌鲁木齐 830063;
2. 新疆农业大学,乌鲁木齐 830052

收稿日期:2019-05-08 出版日期:2019-07-20 发布日期:2019-09-05
通信作者: 武运(1965-),女,新疆乌鲁木齐人,教授,硕士,研究方向为食品工艺与安全,(E-mail)wuyunster@sina.com
作者简介:李晓岩(1981-),男,新疆乌鲁木齐人,工程师,硕士,研究方向为食品检验,(E-mail)28277391@qq.com
基金资助:
国家质量监督检验检疫总局科研项目(2007IK174)

Determination of Malachite Green and Leuco Malachite Green in Cold Water Fish in Xinjiang by UPLC-MS/MS MethodUPLC-MS/MS

LI Xiao-yan¹, WU Yun², WANG Li-ye², SU Min¹, SHEN Hui-hui¹, Bakhetgul Manatbay¹

1. Inspection and Quarantine Technology Center of Xinjiang Entry-Exit Inspection and Quarantine Bureau, Urumqi 830063, China;
2. College of Animal Sciences, Xinjiang Agricultural University, Urumqi 830052, China

Received:2019-05-08 Online:2019-07-20 Published:2019-09-05
Correspondence author: WU Yun (1965-), female, Urumqi, Professor, master, research direction: the Food Technology and Safety, (E-mail) wuyunster@sina.com
Supported by:
Supported by S & T Research Project of General Administration of Quality Supervision, Inspection and Quarantie of the People's Republic of China (2007IK174)

摘要/Abstract

摘要： 【目的】建立新疆冷水鱼中孔雀石绿(MG)和隐色孔雀石绿(LMG)残留量的超高效液相色谱－串联质谱(UPLC-MS/MS)更为简便、高效的检测方法。【方法】样品经1%冰乙酸-乙腈溶液提取,氨基及SCX(强阳离子交换)固相小柱净化,C18 色谱柱分离,电喷雾串联四极杆质谱的多反应监测扫描模式(MRM)进行检测,并采用内标法定量。【结果】MG和LMG在5.0～100.0 μg/L线性范围内具有良好的线性关系,相关系数分别为:0.999 7(MG)和0.999 2 (LMG)。测定低限(LOQ)为2.0 μg/kg。以空白样品为基体做加标回收,测得MG的回收率在88%～105%,LMG的回收率在85%～110%,相对标准偏差(n=6)均为2.2%～15.3%。【结论】该方法样品前处理简便,回收率高,稳定性好。适用于新疆冷水鱼中MG和LMG残留量的日常检测。

关键词: 超高效液相色谱－串联质谱; 新疆冷水鱼; 孔雀石绿; 隐色孔雀石绿

Abstract: 【Objective】 This project aims to establish a more convenient ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the determination of malachite green (MG) and leuco malachite green (LMG) residues in cold water fish in Xinjiang. 【Method】 The sample was extracted with 1% glacial acetic acid-acetonitrile solution, purified by amino and SCX (strong cation exchange) solid phase cartridges, separated by C18 column, and multi-reaction monitoring scanning mode (MRM) of electrospray ionization tandem mass spectrometry, detected and quantified by internal standard method. 【Result】 MG and LMG had a good linear relationship in the linear range of 5.0-100.0 μg/L, and the correlation coefficients were 0.999,7 (MG) and 0.999,2 (LMG), respectively. The lower limit of determination (LOQ) was 2.0 μg/kg. The test was carried out by adding blank sample as the matrix. The recovery rate of MG was 88%-105%, the recovery rate of LMG was 85%-110%, and the relative standard deviation (n=6) was 2.2%-15.3%. 【Conclusion】 The method has the advantages of simple pretreatment, high recovery rate and good stability, whcih is suitable for routine testing of mg and lmg residues in cold water fish in Xinjiang.

Key words: ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS); Xinjiang cold water fish; malachite green; leuco malachite green

中图分类号:

S911

李晓岩, 武运, 王犁烨, 苏敏, 沈慧慧, 巴哈提古丽·马那提拜. UPLC-MS/MS法测定新疆冷水鱼中孔雀石绿与隐色孔雀石绿[J]. 新疆农业科学, 2019, 56(7): 1325-1332.

LI Xiao-yan, WU Yun, WANG Li-ye, SU Min, SHEN Hui-hui, Bakhetgul Manatbay. Determination of Malachite Green and Leuco Malachite Green in Cold Water Fish in Xinjiang by UPLC-MS/MS MethodUPLC-MS/MS[J]. Xinjiang Agricultural Sciences, 2019, 56(7): 1325-1332.

参考文献 19

[1]	赵长兰. 新疆冷水鱼环保网箱养殖现状及其技术[J]. 中国水产,2018,(12):99-102.ZHAO Chang-lan. (2018).Status and technology of environmental cage culture in cold water fish in Xinjiang [J]. Chinese Journal of Fisheries, (12): 99-102. (in Chinese)
[2]	周明, 李杰.新疆博州冷水鱼产业发展思路探讨[J]. 渔业致富指南,2012,(18):15-18.ZHOU Ming, LI Jie. (2012).Discussion on the development of cold water fish industry in Bozhou, Xinjiang . Guide to Fisheries Getting Rich, (18):15-18. (in Chinese)
[3]	李康柏, 陈润发, 洪瑞申, 等. HPLC－MS /MS同位素内标法测定水体中孔雀石绿、结晶紫及其代谢物[J]. 食品安全导刊,2015,9( 4) :75-78.LI Kang-bai, CHEN Run-fa, HONG Rui-shen, et al. (2015).Determination of malachite green, crystal violet and its metabolites in water by HPLC-MS/MS isotope internal standard method[J]. Food Safety Guide, 9(4): 75-78. (in Chinese)
[4]	孙文芳, 黄薇, 刘祥萍, 等. 超高效液相色谱-质谱联用法测定小龙虾虾肉及虾黄中的孔雀石绿及隐色孔雀石绿[J]. 现代预防医学,2018,45(8):1 475-1 478,1 498.SUN Wen-fang, HUANG Wei, LIU Xiang-ping, et al. (2018). Determination of malachite green and leuco malachite green in crayfish shrimp and shrimp yellow by ultra performance liquid chromatography-mass spectrometry[J]. Modern Preventive Medicine, 45(8): 1,475-1,478,1,498. (in Chinese)
[5]	龙朋飞, 王权, 陈永军. 孔雀石绿毒性及其检测研究进展[J]. 水利渔业,2007,27 (4):1-4.LONG Peng-fei, WANG Quan, CHEN Yong-jun. (2007). Research progress on malachite green toxicity and its detection [J]. Water Resources and Fisheries, 27(4): 1-4. (in Chinese)
[6]	刘桂华, 姜杰, 谢建滨, 等. 同位素内标稀释高效液相色谱-质谱法测定鱼体中的孔雀石绿及其代谢物[J]. 现代预防医学,2006,33(1):124 - 126.LIU Gui-hua, JIANG Jie, XIE Jian-bin, et al. (2006).Determination of malachite green and its metabolites in fish by high performance liquid chromatography-mass spectrometry with isotope internal standard dilution[J]. Modern Preventive Medicine, 33(1): 124 - 126. (in Chinese)
[7]	Rao K V K . (1995).Inhibition of DNA synthesis in primary rat hepatocyte cultures by malachite green: a new liver tumor promoter . Toxicology Letters (Shannon), 81(2-3):107-113.
[8]	邱绪建,林洪,王联珠,等. 孔雀石绿及其代谢物无色孔雀石绿在鲫鱼肌肉中的代谢规律[J]. 中国海洋大学学报 (自然科学版),2006,36(5):745-748.QIU Xu-jian, LIN Hong, WANG Lian-zhu, et al. (2006). Metabolism of Malachite Green and Its Metabolite Colorless Malachite Green in Muscle of Carp[J] . Journal of Ocean University of China (Natural Science Edition), 36(5): 745-748. (in Chinese)
[9]	曲志娜, 李存金, 赵思俊,等. 孔雀石绿及其代谢物在大菱鲆肌肉中的消除规[J]. 中国农学通报,2008,24 (6):491-496.QU Zhi-na, LI Cun-jin, ZHAO Si-jun, et al. (2008).Elimination of malachite green and its metabolites in the muscle of turbot[J]. Chinese Agricultural Science Bulletin, 24(6): 491-496. (in Chinese)
[10]	翟毓秀, 郭莹莹, 耿霞, 等. 孔雀石绿的代谢机理及生物毒性研究进展[J]. 中国海洋大学学报(自然科学版),2007,37 (1):27-32.ZHAI Yu-xiu, GUO Ying-ying, GENG Xia, et al. (2007).Advances in Research on Metabolic Mechanism and Biotoxicity of Malachite Green [J]. Journal of Ocean University of China(Natural Science Ed.), 37(1):27-32. (in Chinese)
[11]	ZHANG Y, YU W, PEI L, et al. (2015).Rapid analysis of malaclute green and leucomalachite green in fish muscles with surface-enhanced resonance Raman scattering . Food Chemistry, 169:80-84.
[12]	NY5071-2002 无公害食品渔用药物使用准则[S].Ministry of Agriculture of the People's Republic of China. NY5071-2002 Guidelines for the Use of Non-polluted Food and Fishery Drugs [J]. Beijing: China Standard Press. (in Chinese)
[13]	中华人民共和国农业部. 中华人民共和国农业部公告第235号[EB/OL].[2002 -12-24].Ministry of Agriculture of the People's Republic of China. Announcement No. 235 of the Ministry of Agriculture of the People's Republic of China [EB/OL]. [2002 -12-24]. (in Chinese)
[14]	高娜, 王文兰, 郭军, 等. 高效液相色谱法测定鳕鱼中孔雀石绿含量的不确定度评定[J]. 食品安全质量检测学报,2019,10(3):653-657.GAO Na, WANG Wen-lan, GUO Jun, et al. (2019).Uncertainty evaluation of malachite green content in carp by high performance liquid chromatography [J]. Journal of Food Safety & Quality, 10(3):653-657. (in Chinese)
[15]	洪波, 袁希平, 万译文, 等. 水中孔雀石绿、结晶紫残留量的同时测定[J]. 食品与机械,2012,28(4):84-86.HONG Bo, YUAN Xi-ping, WAN Yi-wen, et al. (2012).Simultaneous Determination of Residues of Malachite Green and Crystal Violet in Water [J]. Food and Machinery, 28(4): 84-86. (in Chinese)
[16]	梁高道, 麦琦. 气相色谱质谱法确认水产品中的孔雀石绿[J]. 公共卫生与预防医学,2009,20(6):69-71.LIANG Gao-dao, MAI Qi. (2009). Identification of malachite green in aquatic products by gas chromatography-mass spectrometry[J] . Journal of Public Health and Preventive Medicine, 20(6): 69-71. (in Chinese)
[17]	贾涛. 酶联免疫法检测饲料中孔雀石绿的探讨[J]. 饲料与畜牧,2015,(11):64-66.JIA Tao. (2015).Detection of malachite green in feed by enzyme-linked immunosorbent assay[J]. Feed and Livestock, (11): 64-66. (in Chinese)
[18]	吴焕乐, 唐建设, 方娟, 等. PDMS-Ag基底表面增强拉曼光谱技术快速检测鱼肉中孔雀石绿[J]. 分析试验室,2019,38(2):147-151.WU Huan-le, TANG Jian-she, FANG Juan, et al. (2019).Rapid detection of malachite green in fish by PDMS-Ag surface enhanced Raman spectroscopy [J]. Laboratory of Analysis, 38(2): 147-151. (in Chinese)
[19]	Commission of the European Communities. Implementing council directive 96/23/EC concerning the performance of analytical methods and interpretation of results,2002/657/EC. [2008-05-20]. http: // www. Wetgiw. Gov. pl/old/UE/prawo/02? _657/e02657. pdf

UPLC-MS/MS法测定新疆冷水鱼中孔雀石绿与隐色孔雀石绿

Determination of Malachite Green and Leuco Malachite Green in Cold Water Fish in Xinjiang by UPLC-MS/MS MethodUPLC-MS/MS

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