PRIME HLB固相萃取-超高效液相色谱-串联质谱法测定蜂产品中10 种头孢类药物的残留量

doi:10.7506/spkx1002-6630-20190717-224

食品科学 ›› 2020, Vol. 41 ›› Issue (22): 330-336.doi: 10.7506/spkx1002-6630-20190717-224

• 安全检测 • 上一篇

PRIME HLB固相萃取-超高效液相色谱-串联质谱法测定蜂产品中10 种头孢类药物的残留量

章豪，吴银良，张宜文，陈国，江潇潇

（1.宁波市农业科学研究院，农业农村部农产品质量安全风险评估实验室（宁波），浙江宁波 315040；2.北京市计量检测科学研究院，北京 100012）

出版日期:2020-11-25 发布日期:2020-11-26
基金资助:
宁波市科技惠民项目（2017C50014）；宁波市农业重大专项（2015C110004）；宁波市社会发展科技攻关项目（2014C50012）；国家农产品质量安全风险评估重大专项（GJFP20191101；GJFP201801101；GJFP201701101；GJFP201701104；GJFP201601101；GJFP201501201；GJFP2014011）

Determination of Ten Cephalosporin Residues in Bee Products by Ultra-high Performance Liquid ChromatographyTandem Mass Spectrometry Coupled with PRIME HLB Solid Phase Extraction

ZHANG Hao, WU Yinliang, ZHANG Yiwen, CHEN Guo, JIANG Xiaoxiao

(1. Laboratory of Quality and Safety Risk Assessment for Agricultural Products (Ningbo), Ministry of Agriculture and Rural Affairs, Ningbo Academy of Agricultural Sciences, Ningbo 315040, China; 2. Beijing Institute of Metrology, Beijing 100012, China)

Online:2020-11-25 Published:2020-11-26

摘要/Abstract

摘要： 建立蜂产品中10 种头孢类药物（头孢喹肟、头孢噻肟、头孢洛宁、头孢哌酮、头孢匹林、头孢氨苄、头孢乙腈、头孢拉定、去乙酰基头孢匹林、头孢唑啉）残留量的超高效液相色谱-串联质谱测定方法。蜂产品样品中头孢类药物用10%甲酸溶液提取，离心，上清液经Oasis PRIME HLB固相萃取柱净化，氮吹后复溶，进行超高效液相色谱-串联质谱分析。采用Acquity BEH C18色谱柱，以0.1%甲酸溶液-甲醇体系作为流动相进行梯度洗脱，电喷雾离子源正离子模式，多反应离子监测模式检测，基质校准外标法定量。结果表明，10 种头孢类药物在一定质量浓度范围内相关系数（r2）大于0.999，线性关系良好；其中检出限为0.1～1 μg/kg，定量限为0.3～3 μg/kg；阴性蜂产品样品的加标回收率为80.0%～95.5%，相对标准偏差为1.5%～4.8%。该方法检测周期短，准确度和精密度高，能满足多种蜂产品样品中头孢类药物的检测需要。

关键词: 蜂产品；头孢类药物；超高效液相色谱-串联质谱法；Oasis PRIME HLB固相萃取柱

Abstract: An ultra-high performance liquid chromatography-tandem mass spectrometry method for the simultaneous quantitative determination of residues of 10 cephalosporins in bee products, including honey, royal jelly and lyophilized royal jelly powder, was established. The samples were extracted with 10% formic acid solution. After being purified by solid-phase microextraction using an Oasis PRIME HLB cartridge, the extract was blown to dryness under a stream of nitrogen gas and then re-dissolved. The analytes were separated on an Acquity UPLC BEH C18 column with a mixture of 0.1% formic acid solution and methanol as the mobile phase by gradient elution. The analysis was carried out using a positive electrospray ion source in the multiple reaction monitoring mode. The matrix-matched external standard method was applied for the quantitative analysis. There were good linear relationships for 10 cephalosporins in certain concentration ranges, with correlation coefficients of more than 0.999. The limits of detection (LODs) for 10 cephalosporins were 0.1–1 μg/kg, and the limits of quantitation (LOQs) were 0.3–3 μg/kg. The recoveries for the analytes spiked into blank bee products were in the range of 80.0%–95.5%, with relative standard deviations of 1.5%–4.8%. This method was time-saving and suitable for the determination of cephalosporins in different bee products due to its simplicity and reliability.

Key words: bee products; cephalosporins; ultra-high performance liquid chromatography-tandem mass spectrometry; Oasis PRIME HLB cartridge

中图分类号:

S859.8

章豪，吴银良，张宜文，陈国，江潇潇. PRIME HLB固相萃取-超高效液相色谱-串联质谱法测定蜂产品中10 种头孢类药物的残留量[J]. 食品科学, 2020, 41(22): 330-336.

ZHANG Hao, WU Yinliang, ZHANG Yiwen, CHEN Guo, JIANG Xiaoxiao. Determination of Ten Cephalosporin Residues in Bee Products by Ultra-high Performance Liquid ChromatographyTandem Mass Spectrometry Coupled with PRIME HLB Solid Phase Extraction[J]. FOOD SCIENCE, 2020, 41(22): 330-336.

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PRIME HLB固相萃取-超高效液相色谱-串联质谱法测定蜂产品中10 种头孢类药物的残留量

Determination of Ten Cephalosporin Residues in Bee Products by Ultra-high Performance Liquid ChromatographyTandem Mass Spectrometry Coupled with PRIME HLB Solid Phase Extraction

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