乳业科学与技术 ›› 2024, Vol. 47 ›› Issue (2): 0-0.

• 分析检测 •    

基于生物芯片技术的生乳兽药检测方法的验证及其应用

祁兵,陈柔含,杨晓君,江春铃,马颖清,邓波   

  1. 上海市农产品质量安全中心
  • 收稿日期:2024-04-16 修回日期:2024-05-22 出版日期:2024-03-01 发布日期:2024-06-18
  • 通讯作者: 邓波
  • 基金资助:
    都市奶业质量安全关键技术研究与集成应用

Verification and application of raw milk veterinary drug detection method based on biochip technology

  • Received:2024-04-16 Revised:2024-05-22 Published:2024-03-01 Online:2024-06-18

摘要: 为验证生物芯片技术在生乳兽药检测方面的检测效果并进行推广应用,本研究针对80种常见兽药,采用生物芯片快速检测法对生乳样品进行检测,并同时采用高效液相色谱-串联质谱法确认。结果表明,生物芯片法检出限符合国家标准检出限要求,且部分优于国家标准;该方法线性范围宽,相关系数(r)均>0.99,线性范围内呈良好的相关性;通过阴性样品加标回收,对加入2倍与4倍检出限的标准样品进行测定,回收率为70%~130%,变异系数(CV值)为5%~10%。该方法前处理简单、检测周期短、灵敏度高、通量大,适合大批量样品的快速筛查。利用以上方法,本研究对2022~2023年,采自上海辖区内的100批次生乳进行检测,检出含有兽药残留的生乳共10批,其中链霉素检出4批(检出值5.86~10.26 μg/kg),磺胺吡啶检出3批(检出值1.09~1.42 μg/kg),磺胺间二甲氧嘧啶检出2批(检出值1.38~1.46 μg/kg),阿维菌素检出1批(检出值1.75 μg/kg)。以上检出值均远低于国际组织、农业农村部公告或国家标准限量规定,本市生乳质量安全总体良好,虽有检出,但均不会造成危害。

关键词: 生物芯片, 生乳, 高效液相色谱-串联质谱法, 质量安全

Abstract: In order to verify the detection effect of biochip technology in the detection of veterinary drugs in raw milk and promote its application, 80 kinds of common veterinary drugs were detected by biochip rapid detection method, and confirmed by high performance liquid chromatography-tandem mass spectrometry. The results showed that the detection limit of the biochip method met the requirements of the national standard, and some of them were better than the national standard. The linear range of the method was wide, the correlation coefficient ( r ) was > 0.99, and there was a good correlation in the linear range. Through the recovery of negative samples, the standard samples with 2 times and 4 times the detection limit were determined. The recovery rate was 70 % ~ 130 %, and the coefficient of variation ( CV value ) was 5 % ~ 10 %.The method has the advantages of simple pretreatment, short detection cycle, high sensitivity and large flux, which is suitable for rapid screening of large quantities of samples. Using the above methods, 100 batches of raw milk collected from Shanghai area from 2022 to 2023 were detected, and 10 batches of raw milk containing veterinary drug residues were detected, including 4 batches of streptomycin ( detection value 5.86~10.26 μg/kg ), 3 batches of sulfapyridine ( detection value 1.09~1.42 μg/kg ), 2 batches of sulfamonomethoxine ( detection value 1.38~1.46 μg/kg ), and 1 batches of avermectin ( detection value 1.75 μg/kg ).The above detection values are far lower than the announcements of international organizations, the Ministry of Agriculture and Rural Affairs or the national standard limit regulations. The quality and safety of raw milk in this city is generally good. Although these veterinary drugs have been detected, they will not cause harm to the human body.

Key words: biochip, raw milk, High performance liquid chromatography-tandem mass spectrometry, quality and safety