| 固相萃取-超高效液相色谱串联质谱测定茶产品中吡蚜酮 |
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| 引用本文： | 余焕,周利,林琴,杨洁,孙荷芝,伍旭东,王新茹,张新忠,陈宗懋,罗逢健.固相萃取-超高效液相色谱串联质谱测定茶产品中吡蚜酮[J].茶叶科学,2019,39(4):440-446. |
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| 作者姓名： | 余焕 周利 林琴 杨洁 孙荷芝 伍旭东 王新茹 张新忠 陈宗懋 罗逢健 |
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| 作者单位： | 中国农业科学院茶叶研究所农产品质量安全研究中心,浙江 杭州 310008;中国农业科学院研究生院,北京 100081;中国农业科学院茶叶研究所农产品质量安全研究中心,浙江 杭州,310008;普洱市质量技术监督综合检测中心,云南 普洱,665099 |
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| 基金项目： | 国家重点研发计划（2016YFD0200207）、浙江省自然科学基金（LY18C160005）、中国农业科学院创新工程（CAAS-ASTIP-TRICAAS） |
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| 摘 要： | 建立了Cleanert PCX固相萃取,超高效液相色谱-串联质谱(UPLC-MS/MS)测定干茶、抹茶和速溶茶粉中吡蚜酮残留量的分析方法。干茶、抹茶和速溶茶粉中的吡蚜酮经甲醇和水的混合溶液提取、Cleanert PCX固相萃取柱富集净化和Acquity BEH C18色谱柱分离后,通过UPLC-MS/MS多反应监测模式(MRM)测定,外标法定量。在0.005~1.000 mg·kg^-1添加范围内,吡蚜酮的平均回收率为77.0%~95.1%,相对标准偏差(RSD,n=5)为1.8%~6.9%,方法的定量限(LOQ)为0.005~0.010 mg·kg^-1。该方法在灵敏度、准确度和回收率上均符合农药残留检测的要求,可为茶产品中吡蚜酮残留量的测定和风险评估提供分析方法。
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| 关 键 词： | 吡蚜酮 茶 农药残留 固相萃取法 高效液相色谱-串联质谱 |
| 收稿时间： | 2018-12-13 |
Determination of Pymetrozine in Tea Products by Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| YU Huan,ZHOU Li,LIN Qin,YANG Jie,SUN Hezhi,WU Xudong,WANG Xinru,ZHANG Xinzhong,CHEN Zongmao,LUO Fengjian.Determination of Pymetrozine in Tea Products by Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Tea Science,2019,39(4):440-446. |
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| Authors: | YU Huan ZHOU Li LIN Qin YANG Jie SUN Hezhi WU Xudong WANG Xinru ZHANG Xinzhong CHEN Zongmao LUO Fengjian |
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| Institution: | 1. Research Center of Quality Safety for Agricultural Products, Tea Research Institute, Chinese Academy of Agricultural Sciences, Hangzhou 310008,China; 2. Graduate School of Chinese Academy of Agricultural Sciences, Beijing 100081, China; 3. Pu'er Comprehensive Technical Testing Center, Pu'er 665099, China |
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| Abstract: | An analytical method for the determination of pymetrozine residues in tea products, including dry tea, matcha and instant tea powder, was established based on Cleanert PCX solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The residual pymetrozine in dry tea, matcha and instant tea powder was extracted by a mixture of methanol and water, cleaned up and concentrated by a Cleanert PCX SPE column, and separated on an Acquity BEH C18 column. Pymetrozine level was detected by UPLC-MS/MS on multiple reaction monitoring (MRM) mode and quantified with external standard method. In the spiked range of 0.005-1.000 mg·kg-1, the average recovery of pymetrozine was 77.0%-95.1%, and the relative standard deviation (RSD, n=5) ranged from 1.8%-6.9%. The limit of quantitation (LOQ) was 0.005 to 0.010 mg·kg-1. The sensitivity, precision and recovery of the developed method meet the requirements for residual pesticides analysis in various tea products. The results of this study can provide an analytical method for the determination and risk assessment of pymetrozine in tea products. |
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| Keywords: | pymetrozine tea pesticide residue solid phase extraction UPLC-MS/MS |
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