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畜禽产品中甲氧苄啶残留检测的方法研究OA

Method development for the detection of trimethoprim residues in livestock and poultry products

中文摘要英文摘要

为提高畜禽产品中甲氧苄啶(trimethoprim,TMP)残留检测的工作效率,开发一种高效液相色谱-串联质谱(high-performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)结合通过式固相萃取(pass-through solid-phase extraction,SPE)方式,测定畜禽产品中TMP残留的检测方法.畜肉和禽蛋样品经酸化乙腈-水体系提取,Na2SO4盐析,EMR-Lipid固相萃取柱净化,经ZORBAX Eclipse Plus C18色谱柱分离,电喷雾离子源在正离子多反应监测模式下测定,外标法定量.结果表明,TMP在畜肉1~20 μg/L、禽蛋0.25~5.0 μg/L的质量浓度范围内线性关系良好,相关系数均大于0.99;畜肉中检出限(limit of detection,LOD)为0.5 μg/kg,定量限(limit of quantification,LOQ)为1.0 μg/kg;禽蛋中LOD为0.1 μg/kg,LOQ为0.2 μg/kg;在畜肉基质的低、中、高质量浓度加标水平测试中,TMP的加标回收率处于70%~120%,相对标准偏差(RSD)≤15%;在禽蛋基质中的回收率处于60%~120%,RSD≤20%;与标准方法进行检测对比,结果经统计学分析和t检验,P值均大于0.05,检测结果无统计学显著差异,满足方法等效验证要求.研究为兽药残留监管与食品安全管控提供有力技术支撑.

To improve the efficiency of trimethoprim(TMP)residue detection in livestock and poultry products,an analytical method was developed using high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)combined with pass-through solid-phase extraction(SPE)for the determination of TMP residues.Meat and egg samples were extracted with acidified acetonitrile-water,salted out with Na2SO4,and purified using EMR-Lipid SPE cartridges.Chromatographic separation was performed on a ZORBAX Eclipse Plus C18 column,and detection was carried out using electrospray ionization in positive ion mode under multiple reaction monitoring,with quantification by external standard method.The results demonstrated good linearity for TMP in the ranges of 1-20 μg/L for meat and 0.25-5.0 μg/L for eggs,with correlation coefficients larger than 0.99.The limits of detection(LOD)were 0.5 μg/kg for meat and 0.1 μg/kg for eggs,and the limits of quantification(LOQ)were 1.0 μg/kg for meat and 0.2 μg/kg for eggs.At low,medium,and high spiking levels,the recoveries of TMP ranged from 70%to 120%with relative standard deviations(RSD)≤15%in meat matrices,and from 60%to 120%with RSD≤20%in egg matrices.Compared with the standard method,statistical analysis and t-test showed P>0.05,indicating no statistically significant difference and confirming that the method meets the requirements for method equivalence validation.This study provides robust technical support for veterinary drug residue monitoring and food safety control.

王佳琪;萨仁图雅;谷永丽;皇金龙;包阿如那;闫炜

呼伦贝尔市农畜产品质量安全中心/呼伦贝尔市农牧业检验检测中心,内蒙古 呼伦贝尔 021008新巴尔虎右旗草原事业发展中心,内蒙古 呼伦贝尔 021309呼伦贝尔市农畜产品质量安全中心/呼伦贝尔市农牧业检验检测中心,内蒙古 呼伦贝尔 021008呼伦贝尔市农畜产品质量安全中心/呼伦贝尔市农牧业检验检测中心,内蒙古 呼伦贝尔 021008呼伦贝尔市农畜产品质量安全中心/呼伦贝尔市农牧业检验检测中心,内蒙古 呼伦贝尔 021008兴安盟现代畜牧业试验区创建服务中心,内蒙古 兴安盟 137000

轻工纺织

畜禽产品高效液相色谱-串联质谱甲氧苄啶

livestock and poultry productshigh-performance liquid chromatography-tandem mass spectrometrytrimethoprim

《包装与食品机械》 2026 (4)

80-88,9

10.3969/j.issn.1005-1295.2026.04.008

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