为验证生物芯片技术在生乳兽药检测方面的效果并进行推广应用,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(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)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;该方法线性范围较宽,相关系数均＞0.99,线性范围内呈良好的相关性;通过阴性样品加标回收实验,对加入2倍与4倍检出限的标准样品进行测定,加标回收率为70％～130％,变异系数为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.利用以上方法对2022-2023年采自上海辖区内的100批次生乳进行检测发现,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),经过国标方法确证,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.生物芯片法相较于传统的HPLC-MS/MS法具有灵敏度高、线性范围宽和检测速度快等优势,可作为生乳兽药残留快速检测的补充手段,具有较高的应用价值.
Verification and Application of Biochip for Detection of Veterinary Drug Residues in Raw Milk
In order to verify the efficacy of biochip technology in the detection of veterinary drug residues in raw milk and to promote its application,80 common veterinary drugs in raw milk were detected by biochip and confirmed by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The results showed that the limit of detection(LOD)of the biochip method met the requirements of the national standard,and the LOD for some veterinary drugs was below the national standard limits.The linear range of the method was wide,with correlation coefficient(r)greater than 0.99.Recoveries for negative samples spiked at 2 × and 4 × LOD concentrations were 70％-130％,with coefficient of variation(CV)of 5％-10％.This method has the advantages of simple pretreatment,short detection period and high sensitivity and is suitable for rapid screening of large quantities of samples.Using the proposed method,10 of 100 batches of raw milk collected from Shanghai during 2022-2023 were tested positive for veterinary drug residues.Streptomyci was detected in 4 batches at concentration levels of 5.86-10.26 μg/kg,sulfapyridine in 3 batches at 1.09-1.42 μg/kg,sulfamonomethoxine in 2 batches at 1.38-1.46 μg/kg,and avermectin in 1 batch at 1.75 μg/kg.These concentration levels were far lower than the maximum residue limits set by international organizations,an announcement of the Ministry of Agriculture and Rural Affairs,and the national standard.Compared with traditional HPLC-MS/MS,the biochip method has the advantages of high sensitivity,wide linear range and fast detection rate.It can be used as a supplementary means for rapid detection of veterinary drug residues in raw milk,and has high application value.
biochipraw milkhigh performance liquid chromatography-tandem mass spectrometryquality and safety
万方数据
维普
