分散固相萃取-超高效液相色谱-串联质谱法测定农产品中乙拌磷及其代谢物
O658; 基于超高效液相色谱-串联质谱(UHPLC-MS/MS)建立定量分析乙拌磷及其5个代谢物(乙拌磷砜、乙拌磷亚砜、内吸磷-S、内吸磷-S-砜、内吸磷-S-亚砜)的方法,应用该方法分析其在农产品(豌豆、芦笋、小麦、咖啡豆和花生)中的残留量.对样品前处理及色谱条件进行优化,样品经过乙腈涡旋提取(小麦、咖啡豆和花生先加水润湿),经盐析分层,取上清液经50 mg C18、50 mg PSA和50 mg NH2混合分散固相萃取净化后,经Thermo Syncronis C18色谱柱(150 mm×2.1 mm,5μm)分离,柱温40℃,进样量2μL,以水和乙腈为流动相梯度洗脱后,采用ESI源,在...
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| Published in | Sepu Vol. 40; no. 2; pp. 130 - 138 |
|---|---|
| Main Authors | , , , , , |
| Format | Journal Article |
| Language | Chinese English |
| Published |
No. 457, Zhongshan Road, Shahekou District, Dalian City, Liaoning Province
上海市农业科学院农药安全评价研究中心,上海市农业科学院农产品质量标准与检测技术研究所,上海 201106
08.02.2022
Editorial board of Chinese Journal of Chromatography |
| Subjects | |
| Online Access | Get full text |
| ISSN | 1000-8713 |
| DOI | 10.3724/SP.J.1123.2021.04028 |
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| Abstract | O658; 基于超高效液相色谱-串联质谱(UHPLC-MS/MS)建立定量分析乙拌磷及其5个代谢物(乙拌磷砜、乙拌磷亚砜、内吸磷-S、内吸磷-S-砜、内吸磷-S-亚砜)的方法,应用该方法分析其在农产品(豌豆、芦笋、小麦、咖啡豆和花生)中的残留量.对样品前处理及色谱条件进行优化,样品经过乙腈涡旋提取(小麦、咖啡豆和花生先加水润湿),经盐析分层,取上清液经50 mg C18、50 mg PSA和50 mg NH2混合分散固相萃取净化后,经Thermo Syncronis C18色谱柱(150 mm×2.1 mm,5μm)分离,柱温40℃,进样量2μL,以水和乙腈为流动相梯度洗脱后,采用ESI源,在正离子扫描和多反应监测(MRM)模式下检测,外标法定量.结果表明,乙拌磷及其代谢物在2.0～200.0μg/L范围内线性关系良好,相关系数(R2)≥0.9981.方法的检出限(LOD)为0.02～2.0μg/kg,并以最小添加水平5μg/kg为定量限(LOQ).乙拌磷及其代谢物在豌豆、芦笋、小麦、咖啡豆和花生中5、100、1000μg/kg 3个添加水平下的平均回收率为75.0％～110.0％,相对标准偏差(RSD)为0.7％～14.9％,方法的准确度和精密度符合农药残留测定.应用建立的方法对市售的40份小麦样品和40份花生样品进行检测,均低于方法的检出限.该方法具有操作简单、快速、灵敏、准确的特点,适用于谷物、油料、蔬菜等多种农产品中乙拌磷及其代谢物的残留检测. |
|---|---|
| AbstractList | O658; 基于超高效液相色谱-串联质谱(UHPLC-MS/MS)建立定量分析乙拌磷及其5个代谢物(乙拌磷砜、乙拌磷亚砜、内吸磷-S、内吸磷-S-砜、内吸磷-S-亚砜)的方法,应用该方法分析其在农产品(豌豆、芦笋、小麦、咖啡豆和花生)中的残留量.对样品前处理及色谱条件进行优化,样品经过乙腈涡旋提取(小麦、咖啡豆和花生先加水润湿),经盐析分层,取上清液经50 mg C18、50 mg PSA和50 mg NH2混合分散固相萃取净化后,经Thermo Syncronis C18色谱柱(150 mm×2.1 mm,5μm)分离,柱温40℃,进样量2μL,以水和乙腈为流动相梯度洗脱后,采用ESI源,在正离子扫描和多反应监测(MRM)模式下检测,外标法定量.结果表明,乙拌磷及其代谢物在2.0～200.0μg/L范围内线性关系良好,相关系数(R2)≥0.9981.方法的检出限(LOD)为0.02～2.0μg/kg,并以最小添加水平5μg/kg为定量限(LOQ).乙拌磷及其代谢物在豌豆、芦笋、小麦、咖啡豆和花生中5、100、1000μg/kg 3个添加水平下的平均回收率为75.0％～110.0％,相对标准偏差(RSD)为0.7％～14.9％,方法的准确度和精密度符合农药残留测定.应用建立的方法对市售的40份小麦样品和40份花生样品进行检测,均低于方法的检出限.该方法具有操作简单、快速、灵敏、准确的特点,适用于谷物、油料、蔬菜等多种农产品中乙拌磷及其代谢物的残留检测. 基于超高效液相色谱-串联质谱(UHPLC-MS/MS)建立定量分析乙拌磷及其5个代谢物(乙拌磷砜、乙拌磷亚砜、内吸磷- S 、内吸磷- S -砜、内吸磷- S -亚砜)的方法,应用该方法分析其在农产品(豌豆、芦笋、小麦、咖啡豆和花生)中的残留量。对样品前处理及色谱条件进行优化,样品经过乙腈涡旋提取(小麦、咖啡豆和花生先加水润湿),经盐析分层,取上清液经50 mg C 18 、50 mg PSA和50 mg NH 2 混合分散固相萃取净化后,经Thermo Syncronis C 18 色谱柱(150 mm×2.1 mm, 5 μm)分离,柱温40 ℃,进样量2 μL,以水和乙腈为流动相梯度洗脱后,采用ESI源,在正离子扫描和多反应监测(MRM)模式下检测,外标法定量。结果表明,乙拌磷及其代谢物在2.0~200.0 μg/L范围内线性关系良好,相关系数( R 2 )≥0.9981。方法的检出限(LOD)为0.02~2.0 μg/kg,并以最小添加水平5 μg/kg为定量限(LOQ)。乙拌磷及其代谢物在豌豆、芦笋、小麦、咖啡豆和花生中5、100、1000 μg/kg 3个添加水平下的平均回收率为75.0%~110.0%,相对标准偏差(RSD)为0.7%~14.9%,方法的准确度和精密度符合农药残留测定。应用建立的方法对市售的40份小麦样品和40份花生样品进行检测,均低于方法的检出限。该方法具有操作简单、快速、灵敏、准确的特点,适用于谷物、油料、蔬菜等多种农产品中乙拌磷及其代谢物的残留检测。 |
| Author | 孙强 唐红霞 温广月 李玉博 董茂锋 王伟民 |
| AuthorAffiliation | 上海市农业科学院农药安全评价研究中心,上海市农业科学院农产品质量标准与检测技术研究所,上海 201106 |
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| Author_FL | DONG Maofeng TANG Hongxia LI Yubo SUN Qiang WANG Weimin WEN Guangyue |
| Author_FL_xml | – sequence: 1 fullname: SUN Qiang – sequence: 2 fullname: LI Yubo – sequence: 3 fullname: WEN Guangyue – sequence: 4 fullname: WANG Weimin – sequence: 5 fullname: DONG Maofeng – sequence: 6 fullname: TANG Hongxia |
| Author_xml | – sequence: 1 fullname: 孙强 – sequence: 2 fullname: 李玉博 – sequence: 3 fullname: 温广月 – sequence: 4 fullname: 王伟民 – sequence: 5 fullname: 董茂锋 – sequence: 6 fullname: 唐红霞 |
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| Keywords | 超高效液相色谱-串联质谱;分散固相萃取;乙拌磷;代谢物;农产品 |
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| Title | 分散固相萃取-超高效液相色谱-串联质谱法测定农产品中乙拌磷及其代谢物 |
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