重庆市蜂产品中31种农兽药残留检测方法开发及其膳食暴露风险评估
TS251; 该研究建立了蜂产品中31种农兽药残留的超高效液相色谱-串联质谱(UPLC-MS/MS)测定方法,分析来源于重庆市各区县的206个蜂产品中的农兽药残留并评估其膳食暴露风险.结果表明,样品用体积分数80％乙腈-水(含0.2％甲酸)提取后,经Oasis PRiME HLB固相萃取柱净化,滤出流速1滴/s;采用Waters ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7 μm)分离,以甲醇和5 mmol/L乙酸铵-0.1％甲酸-水溶液为流动相梯度洗脱,电喷雾离子源,正负离子切换的多反应监测(MRM)模式结合外标法进行定性、定量分析.在此条件下,25种兽...
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| Published in | 中国酿造 Vol. 44; no. 2; pp. 273 - 280 |
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| Main Authors | , , , , |
| Format | Journal Article |
| Language | Chinese |
| Published |
重庆三峡学院生物与食品工程学院,重庆 404100
25.02.2025
重庆市万州食品药品检验所三峡库区道地药材开发利用重庆市重点实验室,重庆 404100%重庆三峡学院生物与食品工程学院,重庆 404100%重庆市万州食品药品检验所三峡库区道地药材开发利用重庆市重点实验室,重庆 404100 |
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| Online Access | Get full text |
| ISSN | 0254-5071 |
| DOI | 10.11882/j.issn.0254-5071.2025.02.041 |
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| Abstract | TS251; 该研究建立了蜂产品中31种农兽药残留的超高效液相色谱-串联质谱(UPLC-MS/MS)测定方法,分析来源于重庆市各区县的206个蜂产品中的农兽药残留并评估其膳食暴露风险.结果表明,样品用体积分数80％乙腈-水(含0.2％甲酸)提取后,经Oasis PRiME HLB固相萃取柱净化,滤出流速1滴/s;采用Waters ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7 μm)分离,以甲醇和5 mmol/L乙酸铵-0.1％甲酸-水溶液为流动相梯度洗脱,电喷雾离子源,正负离子切换的多反应监测(MRM)模式结合外标法进行定性、定量分析.在此条件下,25种兽药及6种农药分别在0.2～100 ng/mL、1.0～250 ng/mL范围内线性关系良好(R2＞0.99),检出限为0.006～0.057 μg/kg,定量限为0.021～0.191 μg/kg,加标回收率为60.3％～116.7％,精密度试验结果的相对标准偏差(RSD)为0.3％～13.2％,说明该方法准确度高且重复性好,适用于蜂产品中农兽药残留的检测.从市售蜂产品样品中共检出19种农兽药残留,其中恩诺沙星、甲氧苄啶、洛硝哒唑、环丙沙星、氯霉素、甲硝唑的食品安全指数(IFS)＞1,膳食暴露风险较高,应加强监管.该结果可为重庆市蜂产品质量监管提供参考. |
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| AbstractList | TS251; 该研究建立了蜂产品中31种农兽药残留的超高效液相色谱-串联质谱(UPLC-MS/MS)测定方法,分析来源于重庆市各区县的206个蜂产品中的农兽药残留并评估其膳食暴露风险.结果表明,样品用体积分数80％乙腈-水(含0.2％甲酸)提取后,经Oasis PRiME HLB固相萃取柱净化,滤出流速1滴/s;采用Waters ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7 μm)分离,以甲醇和5 mmol/L乙酸铵-0.1％甲酸-水溶液为流动相梯度洗脱,电喷雾离子源,正负离子切换的多反应监测(MRM)模式结合外标法进行定性、定量分析.在此条件下,25种兽药及6种农药分别在0.2～100 ng/mL、1.0～250 ng/mL范围内线性关系良好(R2＞0.99),检出限为0.006～0.057 μg/kg,定量限为0.021～0.191 μg/kg,加标回收率为60.3％～116.7％,精密度试验结果的相对标准偏差(RSD)为0.3％～13.2％,说明该方法准确度高且重复性好,适用于蜂产品中农兽药残留的检测.从市售蜂产品样品中共检出19种农兽药残留,其中恩诺沙星、甲氧苄啶、洛硝哒唑、环丙沙星、氯霉素、甲硝唑的食品安全指数(IFS)＞1,膳食暴露风险较高,应加强监管.该结果可为重庆市蜂产品质量监管提供参考. |
| Abstract_FL | An ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was established for the determination of 31 pesticide and veterinary drug residues in bee products,and then the residues were analyzed in 206 bee products from various districts and coun-ties in Chongqing,as well as their dietary exposure risk was assessed.The results showed that samples were extracted with 80％acetonitrile-water(containing 0.2％formic acid),purified by Oasis PRiME HLB solid phase extraction column at the filtration rate of 1 drip/s,separated with Waters ACQUITY UPLC BEH C18 column(100 mm×2.1 mm,1.7 μm)using methanol and 5 mmol/L ammonium acetate-0.1％formic acid-water solution as the mobile phase for gradient elution,qualified using multiple reaction monitoring(MRM)mode with electrospray ionization in positive and negative ion mode,and quantified with external standard method.Under these conditions,the 25 veterinary drug and 6 pesticides residues showed good linear relationships in the range of0.2-250 ng/ml and 1.0-250 ng/ml,respectively(R2＞0.99),their detection limits,quantitation limits,standard recovery rates and relative standard deviations of precision tests results were 0.006-0.057 μg/kg,0.021-0.191 μg/kg,60.3％-116.7％,and 0.3％-13.2％,respectively,indi-cating that the method had high accuracy and good repeatability,and was suitable for the determination of the pesticide and veterinary drug residues in bee products.A total of 19 pesticide and veterinary drug residues were detected in commercially available bee products,among which the food safety index(IFS)of enrofloxacin,trimethoprim,lomidazole,ciprofloxacin,chloramphenicol and metronidazole were greater than 1,indicating a high risk of dietary exposure and should be strengthened supervision.The results provided references for bee products quality supervision in Chongqing. |
| Author | 贺灵芝 阎睿 张华 伍蓉 谭美玲 |
| AuthorAffiliation | 重庆市万州食品药品检验所三峡库区道地药材开发利用重庆市重点实验室,重庆 404100%重庆三峡学院生物与食品工程学院,重庆 404100%重庆市万州食品药品检验所三峡库区道地药材开发利用重庆市重点实验室,重庆 404100;重庆三峡学院生物与食品工程学院,重庆 404100 |
| AuthorAffiliation_xml | – name: 重庆市万州食品药品检验所三峡库区道地药材开发利用重庆市重点实验室,重庆 404100%重庆三峡学院生物与食品工程学院,重庆 404100%重庆市万州食品药品检验所三峡库区道地药材开发利用重庆市重点实验室,重庆 404100;重庆三峡学院生物与食品工程学院,重庆 404100 |
| Author_FL | ZHANG Hua WU Rong TAN Meiling YAN Rui HE Lingzhi |
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| Keywords | dietary exposure risk assessment 农兽药残留 pesticide and veterinary drug residue 蜂产品 bee product UPLC-MS/MS 超高效液相色谱串联质谱 膳食暴露风险评估 |
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| Publisher | 重庆三峡学院生物与食品工程学院,重庆 404100 重庆市万州食品药品检验所三峡库区道地药材开发利用重庆市重点实验室,重庆 404100%重庆三峡学院生物与食品工程学院,重庆 404100%重庆市万州食品药品检验所三峡库区道地药材开发利用重庆市重点实验室,重庆 404100 |
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| Title | 重庆市蜂产品中31种农兽药残留检测方法开发及其膳食暴露风险评估 |
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