气相色谱-四极杆飞行时间质谱快速筛查紫甘蓝中406种农药残留及其在欧盟能力验证中的应用
目的 建立气相色谱-四极杆/飞行时间质谱法(gas chromatography-quadrupole-time of flight-mass spectrometry, GC-QTOF/MS)测定紫甘蓝中406种农药残留的分析方法。方法 采用1%(V/V)乙酸乙腈溶液对紫甘蓝样品均质提取, 4 g无水硫酸镁和1 g氯化钠盐析, 通过自动固相萃取装置使用Carbon/NH2柱净化。应用GC-QTOF/MS在全扫描模式下采集数据, 优化共流出得分和提取特征离子数等筛查参数, 在最佳筛查参数下, 将采集得到的数据与数据库软件(PCDL Manager)中化合物信息比对进行筛查。结果 方法的筛查限(screening detection limits, SDLs)范围为1~50 μg/kg, 定量限(limits of quantification, LOQs)范围为5~50 μg/kg, 在1倍LOQ、2倍LOQ和10倍LOQ3个添加水平下, 平均回收率范围分别为62.7%~119.6%、69.7%~119.6%和64.6%~119.8%, 相对标准偏差范围分别是1.0%~17.8%、0.1%~18.4%和1.0%~18.2%, 在相应的浓度范围内, 406种农药的线性相关系数(r)不小于0.99。同时应用该方法对2019年欧盟能力验证(european union proficiency test ,EUPT)的紫甘蓝样品进行农药残留检测, 检出了所有农药, 并获得A类实验室的评价。结论 该方法准确、可靠, 适用于紫甘蓝等色素较多的碱性样品中农药多残留筛查。
Objective To establish a method for the determination of 406 pesticide residue in red cabbage samples by gas chromatography-quadrupole-time of flight-mass spectrometry (GC-QTOF/MS). Methods Red cabbage samples were extracted by acetonitrile/acetic acid (99:1, V/V) solution with salting-out by anhydrous magnesium sulfate and sodium chloride, and then cleaned-up by Carbon/NH2 through automatic solid phase extraction device. The pesticide residues in the extractants were then analyzed by GC-QTOF/MS in scan mode. The coelution score and number of most specific ions from spectra in data processing were optimized, and under the optimal parameters, the pesticide residues were screened with PCDL. Results The screening detection limits (SDLs) were in the range of 1?50 μg/kg and the limits of quantification (LOQs) were in the range of 5?50 μg/kg. In the spiked concentration of LOQ, 2 LOQ and 10 LOQ, the recoveries were in the range of 62.7%?119.6%, 69.7%?119.6% and 64.6%-119.8% with relative standard deviations (RSDs) in the range of 1.0%?17.8%, 0.1%-18.4% and 1.0%?18.2%, respectively. The correlation coefficients of linear regression equation (r) were all greater than 0.99 in the corresponding linear range for the 406 pesticides. The proposed method was applied to analyze red cabbage sample of European Union Proficiency Test in 2019, and the qualitative and quantitative results were found to be satisfactory and had been classified as class A. Conclusion The proposed method is accurate and reliable, which is suitable for screening pesticide residues in alkaline samples with high level of anthocyanin content, such as red cabbage.
标题：气相色谱-四极杆飞行时间质谱快速筛查紫甘蓝中406种农药残留及其在欧盟能力验证中的应用
英文标题：Simultaneous screening and confirmation of 406 pesticide residues in red cabbage by gas chromatography-quadrupole-time of flight-mass spectrometry and the application in European Union proficiency test
作者：
谢瑜杰 中国检验检疫科学研究院
盖丽娟 北京合众恒星检测科技有限公司
徐凤华 北京合众恒星检测科技有限公司
吴兴强 中国检验检疫科学研究院
范春林 中国检验检疫科学研究院
陈辉 中国检验检疫科学研究院
王雯雯 安捷伦科技(中国)有限公司
吕美玲 安捷伦科技(中国)有限公司
中文关键词:紫甘蓝,农药残留,气相色谱-四极杆/飞行时间质谱法,筛查,欧盟能力验证,
英文关键词:red cabbage,pesticide residue,gas chromatography quadrupole-time-of-flight mass spectrometry,screening,European Union proficiency test,
发表日期：2020-07-20
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