分散固相萃取-高效液相色谱-串联质谱法测定畜禽肝脏中氟虫腈及其代谢物
O658; 欧洲鸡蛋污染事件爆发后,氟虫腈及其代谢物氟甲腈、氟虫腈砜和氟虫腈亚砜残留受到人们较多关注.该研究通过优化前处理方法和色谱条件,建立了畜禽肝脏中氟虫腈及其代谢物的高效液相色谱-串联质谱测定分析方法.样品经10 mL乙腈提取,150 mg PSA、100 mg C18填料净化后,将提取液直接进样分析,以乙腈和水为流动相进行梯度洗脱,在Agilent ZORBAX SB-C18色谱柱(150 mm×2.1 mm,3.5μm)上进行色谱分离,采用电喷雾离子源,负离子扫描,多反应监测(MRM)模式测定,基质校正曲线,外标法定量.结果表明,氟虫腈及其代谢物在0.1～10μg/L范围内线性关系良...
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| Published in | Sepu Vol. 40; no. 2; pp. 206 - 211 |
|---|---|
| Main Authors | , , , , , , |
| Format | Journal Article |
| Language | Chinese English |
| Published |
No. 457, Zhongshan Road, Shahekou District, Dalian City, Liaoning Province
淮安海关,国家饲料安全检测重点实验室(淮安),江苏淮安 223001%江苏食品药品职业技术学院,江苏淮安 223003
08.02.2022
Editorial board of Chinese Journal of Chromatography |
| Subjects | |
| Online Access | Get full text |
| ISSN | 1000-8713 |
| DOI | 10.3724/SP.J.1123.2021.04007 |
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| Abstract | O658; 欧洲鸡蛋污染事件爆发后,氟虫腈及其代谢物氟甲腈、氟虫腈砜和氟虫腈亚砜残留受到人们较多关注.该研究通过优化前处理方法和色谱条件,建立了畜禽肝脏中氟虫腈及其代谢物的高效液相色谱-串联质谱测定分析方法.样品经10 mL乙腈提取,150 mg PSA、100 mg C18填料净化后,将提取液直接进样分析,以乙腈和水为流动相进行梯度洗脱,在Agilent ZORBAX SB-C18色谱柱(150 mm×2.1 mm,3.5μm)上进行色谱分离,采用电喷雾离子源,负离子扫描,多反应监测(MRM)模式测定,基质校正曲线,外标法定量.结果表明,氟虫腈及其代谢物在0.1～10μg/L范围内线性关系良好,相关系数(r2)均大于0.995,方法的检出限和定量限分别为0.2μg/kg和0.5μg/kg.在0.5、1.0、10.0μg/kg 3个加标水平下,氟虫腈及其代谢物的平均回收率为81.1％～99.8％,相对标准偏差(RSD)为6.1％～11.7％.应用建立的方法对99份畜禽肝脏样品进行检测,在4份样品中检测出氟虫腈砜,测定值为1.25～2.82μg/kg.该方法简单,灵敏度和准确度高,适用于大批量畜禽肝脏样品中氟虫腈及其代谢物残留的日常测定. |
|---|---|
| AbstractList | 欧洲鸡蛋污染事件爆发后,氟虫腈及其代谢物氟甲腈、氟虫腈砜和氟虫腈亚砜残留受到人们较多关注。该研究通过优化前处理方法和色谱条件,建立了畜禽肝脏中氟虫腈及其代谢物的高效液相色谱-串联质谱测定分析方法。样品经10 mL乙腈提取,150 mg PSA、100 mg C18填料净化后,将提取液直接进样分析,以乙腈和水为流动相进行梯度洗脱,在Agilent ZORBAX SB-C18色谱柱(150 mm×2.1 mm, 3.5 μm)上进行色谱分离,采用电喷雾离子源,负离子扫描,多反应监测(MRM)模式测定,基质校正曲线,外标法定量。结果表明,氟虫腈及其代谢物在0.1~10 μg/L范围内线性关系良好,相关系数(
r
2
)均大于0.995,方法的检出限和定量限分别为0.2 μg/kg和0.5 μg/kg。在0.5、1.0、10.0 μg/kg 3个加标水平下,氟虫腈及其代谢物的平均回收率为81.1%~99.8%,相对标准偏差(RSD)为6.1%~11.7%。应用建立的方法对99份畜禽肝脏样品进行检测,在4份样品中检测出氟虫腈砜,测定值为1.25~2.82 μg/kg。该方法简单,灵敏度和准确度高,适用于大批量畜禽肝脏样品中氟虫腈及其代谢物残留的日常测定。 O658; 欧洲鸡蛋污染事件爆发后,氟虫腈及其代谢物氟甲腈、氟虫腈砜和氟虫腈亚砜残留受到人们较多关注.该研究通过优化前处理方法和色谱条件,建立了畜禽肝脏中氟虫腈及其代谢物的高效液相色谱-串联质谱测定分析方法.样品经10 mL乙腈提取,150 mg PSA、100 mg C18填料净化后,将提取液直接进样分析,以乙腈和水为流动相进行梯度洗脱,在Agilent ZORBAX SB-C18色谱柱(150 mm×2.1 mm,3.5μm)上进行色谱分离,采用电喷雾离子源,负离子扫描,多反应监测(MRM)模式测定,基质校正曲线,外标法定量.结果表明,氟虫腈及其代谢物在0.1～10μg/L范围内线性关系良好,相关系数(r2)均大于0.995,方法的检出限和定量限分别为0.2μg/kg和0.5μg/kg.在0.5、1.0、10.0μg/kg 3个加标水平下,氟虫腈及其代谢物的平均回收率为81.1％～99.8％,相对标准偏差(RSD)为6.1％～11.7％.应用建立的方法对99份畜禽肝脏样品进行检测,在4份样品中检测出氟虫腈砜,测定值为1.25～2.82μg/kg.该方法简单,灵敏度和准确度高,适用于大批量畜禽肝脏样品中氟虫腈及其代谢物残留的日常测定. |
| Author | 朱臻怡 冯民 何正和 何健 鲍会梅 黄高明 魏云计 |
| AuthorAffiliation | 淮安海关,国家饲料安全检测重点实验室(淮安),江苏淮安 223001%江苏食品药品职业技术学院,江苏淮安 223003 |
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| Author_FL | HUANG Gaoming HE Zhenghe BAO Huimei FENG Min ZHU Zhenyi HE Jian WEI Yunji |
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| Keywords | 高效液相色谱-串联质谱;分散固相萃取;氟虫腈及其代谢物;畜禽肝脏 |
| Language | Chinese English |
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| Publisher | 淮安海关,国家饲料安全检测重点实验室(淮安),江苏淮安 223001%江苏食品药品职业技术学院,江苏淮安 223003 Editorial board of Chinese Journal of Chromatography |
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| Snippet | O658; 欧洲鸡蛋污染事件爆发后,氟虫腈及其代谢物氟甲腈、氟虫腈砜和氟虫腈亚砜残留受到人们较多关注.该研究通过优化前处理方法和色谱条件,建立了畜禽肝脏中氟虫腈及其代谢物的高效液相色谱-串联质谱测定分析方法.样品经10 mL乙腈提取,150 mg PSA、100 mg... 欧洲鸡蛋污染事件爆发后,氟虫腈及其代谢物氟甲腈、氟虫腈砜和氟虫腈亚砜残留受到人们较多关注。该研究通过优化前处理方法和色谱条件,建立了畜禽肝脏中氟虫腈及其代谢物的高效液相色谱-串联质谱测定分析方法。样品经10 mL乙腈提取,150 mg PSA、100 mg... |
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| Title | 分散固相萃取-高效液相色谱-串联质谱法测定畜禽肝脏中氟虫腈及其代谢物 |
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