Suppr超能文献

[高效液相色谱-串联质谱法测定蜂蜜中9种农药残留]

[Determination of nine pesticide residues in honey using high performance liquid chromatography-tandem mass spectrometry].

作者信息

Zhu Zhitong, Liu Han, Ning Qianqian, Zhang Jian, Shen Weijian, Chen Huilan, Shen Chongyu, Xie Wen

机构信息

Animal, Plant and Food Inspection Center, Nanjing Customs, Nanjing 210019, China.

Hangzhou Customs, Hangzhou 310016, China.

出版信息

Se Pu. 2019 Jan 8;37(1):8-14. doi: 10.3724/SP.J.1123.2018.09007.

Abstract

A method is proposed for the simultaneous determination of nine benzimidazole and neonicotinoid pesticides present in honey by employing automatic solid-phase extraction with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). A honey sample was dissolved in a phosphate buffer (pH=7.8) followed by ultrasonic extraction. The extracts were then purified through solid-phase extraction (SPE) with hydrophilic-lipophilic balance (HLB) cartridges. Finally, nitrogen was blown on the obtained mixture, and the mixture was subsequently filtered for conducting HPLC-MS/MS analysis. Nine compounds were detected under the multiple reaction monitoring (MRM) mode, and the corresponding quantification was performed by employing the method of internal standards. The nine detected pesticides demonstrated good linearity in the range of 0.002-0.05 mg/L, with the correlation coefficient values () being higher than 0.99. The limits of detection (LODs) (=3) and limits of quantification (LOQs) (=10) were found to be in the ranges of 0.1-1.0 μg/kg and 0.3-2.0 μg/kg, respectively. Furthermore, the results indicated that the recoveries of the nine detected pesticides range from 78.2%-101.2% at three spiked levels of 5.0, 10.0, and 20.0 μg/kg with a relative standard deviation (RSD) range of 1.3%-14.3% (=6). Hence, the proposed method is rapid and can be employed for accurate determination of pesticide residues in large quantities of honey samples.

摘要

本文提出了一种采用自动固相萃取结合高效液相色谱 - 串联质谱法(HPLC - MS/MS)同时测定蜂蜜中九种苯并咪唑和新烟碱类农药的方法。将蜂蜜样品溶解于磷酸盐缓冲液(pH = 7.8)中,然后进行超声提取。提取物随后通过使用亲水亲脂平衡(HLB)柱的固相萃取(SPE)进行纯化。最后,对所得混合物进行氮气吹干,随后过滤以进行HPLC - MS/MS分析。在多反应监测(MRM)模式下检测到九种化合物,并采用内标法进行相应的定量分析。所检测的九种农药在0.002 - 0.05 mg/L范围内呈现良好的线性,相关系数值()高于0.99。检测限(LOD,= 3)和定量限(LOQ,= 10)分别在0.1 - 1.0 μg/kg和0.3 - 2.0 μg/kg范围内。此外,结果表明,在5.0、10.0和20.0 μg/kg三个加标水平下,所检测的九种农药的回收率在78.2% - 101.2%之间,相对标准偏差(RSD)范围为1.3% - 14.3%(= 6)。因此,该方法快速,可用于准确测定大量蜂蜜样品中的农药残留。

文献检索

告别复杂PubMed语法,用中文像聊天一样搜索,搜遍4000万医学文献。AI智能推荐,让科研检索更轻松。

立即免费搜索

文件翻译

保留排版,准确专业,支持PDF/Word/PPT等文件格式,支持 12+语言互译。

免费翻译文档

深度研究

AI帮你快速写综述,25分钟生成高质量综述,智能提取关键信息,辅助科研写作。

立即免费体验