摘要
建立一种QuEChERS-同位素-UPLC-MS/MS方法,用于快速测定禽蛋和鸡肉中6种喹诺酮类药物的残留;根据检测数据分析内蒙古地区禽蛋和鸡肉中喹诺酮类药物的污染水平,使用喹诺酮类药物的总危害商数(∑Q_(HQ))评估膳食暴露风险。通过改进QuEChERS前处理技术(提取液、吸附净化剂)、色谱柱和流动相等条件优化实验方法,将优化后的方法应用于233份禽蛋和鸡肉样品。使用T3色谱柱、V(5 mmol/L甲酸铵和0.1%甲酸水)∶V(甲醇)=98∶2和V(5 mmol/L甲酸铵和0.1%甲酸水)∶V(甲醇)=2∶98流动相、Discovery■DSC-18 SPE作吸附剂、V(5 mmol/L甲酸铵和0.1%甲酸水)∶V(乙腈)=2∶98为提取液,6种喹诺酮类药物色谱峰形尖锐,分离效果好,响应值高,在1~100 ng/mL范围内线性关系良好,相关系数R≥0.9990,检出限范围为0.3~1μg/kg,定量限范围为1~3μg/kg,在3个不同加标水平浓度点的回收率范围为88.1%~117.1%,相对标准偏差范围为0.60%~7.19%(n=6)。禽蛋中喹诺酮类药物的检出率为3.33%(4/120),鸡肉中喹诺酮类药物的检出率为6.19%(7/113),总体检出率为4.72%(11/233)。改进后的方法具有较低的检出限和较高的准确度,能够简单快速地测定禽蛋和鸡肉中的喹诺酮类药物残留。在喹诺酮类药物的风险评估中,各年龄组的6种喹诺酮类药物的Q HQ均小于1,各年龄组的总危害商数(∑Q_(HQ))均小于1,风险处于可接受的水平。
A QuEChERS-isotope-UPLC-MS/MS method was developed for the rapid determination of six quinolone residues in poultry eggs and chicken meat.Based on the contamination levels of quinolones detected in poultry eggs and chicken meat in Inner Mongolia region,the dietary exposure risk was evaluated using the total hazard quotient(∑Q_(HQ))of quinolones.The method was optimized by improving the QuEChERS pre-treatment technique(extraction solution and adsorption purification agent),chromatographic column,and mobile phase membrane conditions,and was applied to 233 poultry egg and chicken meat samples.Using a T3 chromatographic column with mobile phases V(5 mmol/L ammonium formate and 0.1%formic acid in water)∶V(methanol)=98∶2 and V(5 mmol/L ammonium formate and 0.1%formic acid in water)∶V(methanol)=2∶98,Discovery■DSC-18 SPE as the adsorbent,an extraction solution of V(5 mmol/L ammonium formate and 0.1%formic acid in water)∶V(acetonitrile)=2∶98,sharp chromatographic peaks,good separation,and strong signal responses were achieved.The six quinolones showed good linearity in the range of 1~100 ng/mL with correlation coefficients R≥0.9990.The detection limits ranged from 0.3~1μg/kg,and the quantification limits ranged from 1 to 3μg/kg.Recoveries at three different spiked levels ranged from 88.1%to 117.1%,and the relative standard deviations(RSDs)ranged from 0.60%to 7.19%(n=6).The detection rate of quinolones was 3.33%(4/120)in poultry eggs and it was 6.19%(7/113)in chicken meat,with an overall detection rate of 4.72%(11/233).The improved method features low detection limits and high accuracy,enabling simple and rapid determination of quinolone residues in poultry eggs and chicken meat.Risk assessment showed that the Q HQ for the six quinolones in all age groups was below 1,and the total hazard quotient(∑Q_(HQ))for all age groups was also less than 1,indicating an acceptable risk exposure level of dietary exposure rate.
作者
陈旭
刘春波
张海燕
包玉兰
张丽敏
赵宏
CHEN Xu;LIU Chun-bo;ZHANG Hai-yan;BAO Yu-lan;ZHANG Li-min;ZHAO Hong(Inner Mongolia Autonomous Region Hospital of Traditional Chinese Medicine,Hohhot 010010,China;Hohhot Center for Disease Control and Prevention,Hohhot 010010,China)
出处
《化学试剂》
2025年第9期81-88,共8页
Chemical Reagents
基金
内蒙古自然科学基金项目(2024FX34)。
关键词
QUECHERS
同位素
超高效液相色谱串联质谱法
喹诺酮类
膳食暴露风险
QuEChERS
isotope
ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
quinolones
dietary exposure risk
