同位素稀释气相色谱-串联质谱法测定动物源食品中克霉唑残留量

韩超; 胡贝贞; 李舟; 朱振瓯; 沈燕; 周秀锦

doi:10.13386/j.issn1002-0306.2020030010

同位素稀释气相色谱-串联质谱法测定动物源食品中克霉唑残留量

韩超¹,
胡贝贞²,
李舟³,
朱振瓯³,
沈燕¹,
周秀锦^4, ,

1. 浙江树人大学生物与环境工程学院, 浙江杭州 310015;
2. 绍兴海关综合技术服务中心, 浙江绍兴 312000;
3. 温州海关综合技术服务中心, 浙江温州 325027;
4. 舟山海关综合技术服务中心, 浙江舟山 316000

基金项目:

浙江树人大学人才引进基金项目（2019R024）。

详细信息

作者简介:
韩超(1977-),男,博士,教授,研究方向:食品质量安全与检测,E-mail:hanchao96@163.com。

通讯作者:
周秀锦(1975-),女,硕士,高级工程师,研究方向:食品质量安全与检测,E-mail:68261222@qq.com。

中图分类号: TS207.3
计量
- 文章访问数: 314
- HTML全文浏览量: 41
- PDF下载量: 28
出版历程
- 收稿日期: 2020-03-01
- 网络出版日期: 2021-03-02
- 刊出日期: 2021-02-28

Determination of Clotrimazole Residue in Animal-Derived Food by Gas Chromatography-Tandem Mass Spectrometry with Isotope Dilution

1. College of Biological and Environmental Engineering, Zhejiang Shuren University, Hangzhou 310015, China;
2. Shaoxing Customs Comprehensive Technical Service Center, Shaoxing 312000, China;
3. Wenzhou Customs Comprehensive Technical Service Center, Wenzhou 325027, China;
4. Zhoushan Customs Comprehensive Technical Service Center, Zhoushan 316000, China

摘要

摘要: 建立了动物源食品（猪肉、鸡肉、猪脂肪、猪心、猪肝、猪肾）中克霉唑残留量的同位素稀释气相色谱-串联质谱（GC-MS/MS）测定方法。样品经加速溶剂提取后，用凝胶渗透色谱净化。采用HP-5 MS色谱柱（30 m×0.25 mm×0.25 μm）进行分离，多反应监测（MRM）模式检测，同位素内标法定量。实验结果表明，克霉唑在1~100 μg/L浓度范围内线性良好，决定系数（R²）为0.9995，定量限（LOQ，S/N≥10）为2.0 μg/kg。在2.0、5.0、20.0 μg/kg加标水平下，回收率在82.6%~116.5%之间，相对标准偏差为5.2%~13.5%。该方法灵敏度高、准确性好，能够满足动物源食品中克霉唑残留量的确证和定量分析。
- 动物源食品 /
- 克霉唑 /
- 残留 /
- 同位素稀释 /
- 气相色谱-串联质谱法
Abstract: An isotope dilution gas chromatography-tandem mass spectrometry(GC-MS/MS)method for the determination of clotrimazole residues in animal-derived food(Pork,chicken,pig fat,pig heart,pig liver,pig kidney)was established. The samples were extracted with accelerated solvent extraction,and cleaned up by gel permeation chromatography. HP-5 MS chromatographic column(30 m×0.25 mm×0.25 μm)was used for separation,multi-reaction monitoring(MRM)mode detection,and isotope internal standard method for quantification. Results showed that there was a good linearity for clotrimazole in the range of 1~100 μg/L with a correlation coefficient(R²)of 0.9995. The limit of quantitation(LOQ,S/N≥10)of the method was 2.0 μg/kg. The average recoveries at three spiking levels(2.0,5.0,20.0 μg/kg)were 82.6%~116.5%. Relative standard deviation(RSD)were 5.2%~13.5%. This method has high sensitivity and accuracy,and can be used for the confirmation and quantitative analysis of clotrimazole residues in animal-originated foodstuffs.
- animal-derived food /
- clotrimazole /
- residue /
- isotope dilution /
- gas chromatography-tandem mass spectrometry

HTML全文

参考文献(18)

[1]	陈忠兰,吴先富,王瑾,等. 克霉唑有关物质检查色谱条件的优化[J]. 药物分析杂志,2019,39(9):1694-1697.
[2]	Dismukes W E. Introduction to antifungal drugs[J]. Clin Infect Dis,2000,30(4):653-657.
[3]	张致平. 抗真菌药物研究进展[J]. 中国处方药,2006(3):28-32.
[4]	王旭,徐颖,高中华,等. 复方克霉唑搽剂中醋酸氟轻松和克霉唑的含量测定[J]. 解放军药学学报,2018,34(5):427-429.
[5]	厉娜,于红燕,姜爱霞. HPLC法测定克霉唑阴道片含量的方法研究[J]. 药学研究,2015,34(5):280-281.
[6]	刘娜,谢子立,吴小英,等. HPLC法测定克霉唑阴道片中咪唑含量的方法研究[J]. 广州化工,2017,45(18):92-94.
[7]	周琳,王伯初. 克霉唑栓含量和有关物质的测定[J]. 中国药业,2011,20(5):22-24.
[8]	何淑旺,王雪敏,谢晓燕,等. HPLC法同时测定克霉唑片中多种有关物质[J]. 药学与临床研究,2016,24(4):315-317.
[9]	李青翠,田方,任瑞莉,等. HPLC法测定克霉唑栓的含量[J]. 药物分析杂志,2009,29(8):1364-1366.
[10]	Assress H A,Nyoni H,Mamba B B,et al. Target quantification of azole antifungals and retrospective screening of other emerging pollutants in wastewater effluent using UHPLC-QTOF-MS[J]. Environmental Pollution,2019,253:655-666.
[11]	张凯,秦宇,卞华,等. QuEChERS-超高效液相色谱-串联质谱法检测羊肉中8种抗真菌药[J]. 色谱,2018,36(10):999-1004.
[12]	Ji Y H,Li X H,Wang Z Z,et al. Extraction optimization of accelerated solvent extraction for eight active compounds from Yaobitong capsule using response surface methodology:Comparison with ultrasonic and reflux extraction[J]. J Chromatogr A,2020,460984.
[13]	Hu D J,Han B X,Chen C W,et al. Determination of seven oligosaccharides and sucrose in Pseudostellaria heterophylla by pressurized liquid extraction and ultra-high performance liquid chromatography with charged aerosol detector and tandem mass spectrometry[J]. J Chromatogr A,2020,1609:460441.
[14]	Ahmad R,Ahmad N,Shehzad A. Solvent and temperature effects of accelerated solvent extraction(ASE)coupled with ultra-high pressure liquid chromatography(UHPLC-DAD)technique for determination of thymoquinone in commercial food samples of black seeds(Nigella sativa)[J]. Food Chem,2020,309:125740.
[15]	Ahmad R,Ahmad N,Al-Anaki WS,et al. Solvent and temperature effect of accelerated solvent extraction(ASE)coupled with ultra-high-pressure liquid chromatography(UHPLC-PDA)for the determination of methyl xanthines in commercial tea and coffee[J]. Food Chem,2020,311:126021.
[16]	Varela-Martínez D A,González-Curbelo M Á,González-Sálamo J,et al. Analysis of multiclass pesticides in dried fruits using QuEChERS-gas chromatography tandem mass spectrometry[J]. Food Chem,2019,297:124961.
[17]	Gaweł M,Kiljanek T,Niewiadowska A,Semeniuk S,et al. Determination of neonicotinoids and 199 other pesticide residues in honey by liquid and gas chromatography coupled with tandem mass spectrometry[J]. Food Chem,2019,282:36-47.
[18]	Rutkowska E,Łozowicka B,Kaczyński P. Three approaches to minimize matrix effects in residue analysis of multiclass pesticides in dried complex matrices using gas chromatography tandem mass spectrometry[J]. Food Chem,2019,279:20-29.

施引文献(8)

期刊类型引用(7)

1.	黄积武，郭思妤，王慧敏，周博文，王昊阳，郭寅龙，刘文. 上海白玉兰花香和鲜花精油挥发性成分的GC-MS分析研究. 化学试剂. 2025(01): 80-85 . 百度学术
2.	叶小真，张龙华，陈红梅，林曦碧，李渊顺，杨晓文，陈全助. 樟树枝枯病病原菌生物学特性及杀菌剂室内筛选. 福建林业科技. 2024(01): 23-32 . 百度学术
3.	刘庆璇，庄连玉，马文局，孙光辉，刘亚辉，李冠喜. 樟树叶片精油对微生物生长的抑制作用. 曲阜师范大学学报(自然科学版). 2023(02): 88-92 . 百度学术
4.	赵纯静，陈卫国，白丽，武有聪. 美洲大蠊提取物CⅡ-3对白假丝酵母菌生物膜形成的作用. 大理大学学报. 2023(04): 28-33 . 百度学术
5.	孙琦，李明珠，安珂瑶，熊馨炜，范爽妍，乐涛. 基于科研项目驱动的食品类专业大学生创新能力培养——以纳米金的绿色制备与性能研究为例. 农产品加工. 2023(21): 150-152 . 百度学术
6.	智亚楠，赵筱岑，汪伟，鲁泽培，王春生，陈利军. 番茄挥发物组分分析及其对番茄灰霉病菌的熏蒸抑菌作用. 化学研究与应用. 2022(09): 2029-2035 . 百度学术
7.	石瑀，张雨佳，任怡琳，陆春雷，王娟娟，江露露，李华祥，高亚军. 牛樟树提取物对食源性致病菌的抑制效果. 食品科技. 2021(04): 168-172+179 . 百度学术