摘要
建立了畜禽肌肉、内脏和牛奶中螺旋霉素I及其代谢物(新螺旋霉素I)残留量的高效液相色谱-串联质谱分析方法。试样经三羟甲基氨基甲烷(Tris)溶液提取,偏磷酸溶液沉淀蛋白,HLB柱净化,C18色谱柱(100 mm×2.1 mm,2.7μm)分离,以乙腈和0.1%甲酸水溶液为流动相梯度洗脱,采用电喷雾离子源正离子扫描,多反应监测(MRM)模式检测,外标法定量。考察了提取溶剂、固相萃取柱、pH值等对加标回收率的影响,优化了色谱条件和质谱参数。结果表明,螺旋霉素I及其代谢物在0.2~20.0μg/L范围内线性关系良好,相关系数(r)大于0.999,方法检出限为10μg/kg,定量下限为50μg/kg。在50~600μg/kg加标浓度下,螺旋霉素I及其代谢物的平均回收率为71.8%~102%,相对标准偏差为1.7%~8.5%。该方法满足食品理化检测要求,适用于畜禽肌肉、内脏和牛奶中螺旋霉素I及其代谢物的同时测定。
A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was established for the determination of spiramycinⅠand its metabolite(neospiramycinⅠ)in livestock and poultry tissues and milk.After extraction of the samples with hydroxymethyl amino⁃methane(Tris)and precipitation of proteins with metaphosphoric acid,the extracts were purified with HLB columns.The extracts were separated on a reversed-phase C18 column(100 mm×2.1 mm,2.7μm)by gradient elution with acetonitrile and 0.1%formic acid aqueous solution.Tandem mass spectrometry with electrospray ionization was used to carry out quantitative analysis in positive ion and multiple reaction monitoring(MRM)mode by external standard method.The extraction solution,the types of SPE columns,and pH of the working solutions were evaluated.The chromatographic con⁃ditions and mass spectrometric parameters were optimized.The results showed that excellent linearity was obtained in the range of 0.2-20.0μg/L with the correlation coefficients(r)higher than 0.999.The limits of detection(LODs)were 10μg/kg and the limits of quantification(LOQs)were 50μg/kg for the target analytes.At spiked levels of 50-600μg/kg,the average recoveries ranged from 71.8%to 102%,with relative standard deviations(RSDs)ranging from 1.7%to 8.5%.The method conforms to the criteria for quality control of veterinary drug residue analysis in foods and can be applied to the simultaneous detection of spiramycinⅠand its metabolite in various matrices,including muscle,viscera,and milk from livestock and poultry.
作者
朱萍萍
岳振峰
祝筱慧
赵凤娟
李丽苏
周海鹏
ZHU Ping-ping;YUE Zhen-feng;ZHU Xiao-hui;ZHAO Feng-juan;LI Li-su;ZHOU Hai-peng(Food Inspection and Quarantine Technology Center of Shenzhen Customs,Shenzhen 518045,China;School of Food and Drug,Shenzhen Polytechnic University,Shenzhen 518055,China;Hangzhou Xinxuan Network Technology Co.,Ltd,Hangzhou 310051,China)
出处
《分析测试学报》
北大核心
2026年第2期406-413,共8页
Journal of Instrumental Analysis
基金
深圳市科技计划(KCXFZ20240903092405007)
国家重点研发计划课题(2017YFC1601603)。
