QuEChERS-超高效液相色谱-串联质谱法测定牛奶中6种头孢菌素类抗生素残留

doi:10.3724/SP.J.1123.2017.11007

色谱 ›› 2018, Vol. 36 ›› Issue (4): 345-350.DOI: 10.3724/SP.J.1123.2017.11007

QuEChERS-超高效液相色谱-串联质谱法测定牛奶中6种头孢菌素类抗生素残留

张小刚, 王霞, 戴春风, 陈美莲

上海市农产品质量安全检测中心, 农业部食品质量监督检验测试中心(上海), 农业部奶产品质量安全风险评估实验室(上海), 上海 201708

收稿日期:2017-11-06 出版日期:2018-04-08 发布日期:2014-02-26
通讯作者: 陈美莲,Tel:(021)59804370,E-mail:13601975089@163.com
基金资助:
公益性行业（农业）科研专项（201403071）.

Determination of six cephalosporin residues in milk by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry

ZHANG Xiaogang, WANG Xia, DAI Chunfeng, CHEN Meilian

Shanghai Agricultural Products Quality and Safety Testing Center, Ministry of Agriculture Food Quality Supervision and Inspection Center(Shanghai), Ministry of Agriculture-Milk Risk Assessment Laboratory(Shanghai), Shanghai 201708, China

Received:2017-11-06 Online:2018-04-08 Published:2014-02-26
Supported by:
Special Public Welfare Industry (Agriculture) Research (No. 201403071).

摘要/Abstract

摘要：

建立了QuEChERS-超高效液相色谱-串联质谱（UPLC-MS/MS）同时测定牛奶中6种头孢菌素类抗生素的分析方法。牛奶样品加入含1%（v/v）醋酸的乙腈溶液提取，于45℃氮吹浓缩，经100 mg C18吸附剂净化后，采用HSS T3柱（100 mm×2.1 mm，1.8 μm）分离，以0.1%（v/v）甲酸水溶液和乙腈为流动相进行梯度洗脱，在电喷雾离子源、正离子模式（ESI⁺）下电离，多反应监测（MRM）模式下检测，外标法定量。结果表明，6种头孢菌素类抗生素在2~200 μg/L质量浓度范围内均呈良好的线性关系，相关系数（r）均大于0.999，方法的检出限为0.2~0.6 μg/kg、定量限为0.8~2.0 μg/kg。在8、16和80 μg/kg的加标水平下，6种头孢菌素类抗生素的回收率为75.1%~94.4%，相对标准偏差为0.63%~8.3%。该方法简单快捷，准确可靠，适用于牛奶中头孢菌素类抗生素残留的同时测定。

关键词: QuEChERS, 超高效液相色谱-串联质谱, 牛奶, 头孢菌素类抗生素

Abstract:

A simple, rapid and sensitive method for the simultaneous determination of six cephalosporin (cephalexin, cephapirin, cefotaxime, cefazolin, cefalonium and cefquinome) residues in milk was developed by QuEChERS coupled with ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).The milk samples were extracted with 10 mL acetonitrile containing 1%(v/v) acetic acid, and then centrifuged for 10 min.The supernatant was cleaned up with 100 mg C18 adsorbent powder.The analytes were separated on a reversed phase HSS T3 column (100 mm×2.1 mm, 1.8 μm) using acetonitrile and water containing 0.1%(v/v) formic acid as mobile phases with gradient elution.An electrospray ionization (ESI) source was used in the multiple reaction monitoring (MRM) mode.The analytes were quantified using an external standard method.The linear relationships of the six cephalosporins were good and the correlation coefficients (r) were greater than 0.999.The limits of detection (LODs) and the limits of quantification (LOQs) for the analytes were in the range of 0.2-0.6 μg/kg and 0.8-2 μg/kg, respectively.The recoveries of the target analytes were between 75.1% and 94.4% at spiked levels of 8, 16, 80 μg/kg.The relative standard deviations (RSDs) were no more than 8.3%(n=6).The method is simple and sensitive, and can be suitable for the analysis of the cephalosporin residues in milk.

Key words: cephalosporins, milk, QuEChERS, ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

中图分类号:

O658

张小刚, 王霞, 戴春风, 陈美莲. QuEChERS-超高效液相色谱-串联质谱法测定牛奶中6种头孢菌素类抗生素残留[J]. 色谱, 2018, 36(4): 345-350.

ZHANG Xiaogang, WANG Xia, DAI Chunfeng, CHEN Meilian. Determination of six cephalosporin residues in milk by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(4): 345-350.

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QuEChERS-超高效液相色谱-串联质谱法测定牛奶中6种头孢菌素类抗生素残留

Determination of six cephalosporin residues in milk by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry

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