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纸质出版日期:2018
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王莹, 魏赫, 乔菲, 等. 气相色谱-串联质谱法快速筛查人参中192种农药残留[J]. 中国实验方剂学杂志, 2018,24(15):83-92.
WANG Ying, WEI He, QIAO Fei, et al. Determination of 192 Pesticide Residues in Ginseng by GC-MS/MS[J]. Chinese journal of experimental traditional medical formulae, 2018, 24(15): 83-92.
王莹, 魏赫, 乔菲, 等. 气相色谱-串联质谱法快速筛查人参中192种农药残留[J]. 中国实验方剂学杂志, 2018,24(15):83-92. DOI: 10.13422/j.cnki.syfjx.20181515.
WANG Ying, WEI He, QIAO Fei, et al. Determination of 192 Pesticide Residues in Ginseng by GC-MS/MS[J]. Chinese journal of experimental traditional medical formulae, 2018, 24(15): 83-92. DOI: 10.13422/j.cnki.syfjx.20181515.
目的:利用气相色谱-串联质谱(GC-MS/MS)检测技术,建立了人参中192种农药多残留的快筛方法,并对11批样品(包括西洋参、人参、红参、生晒参)进行测定。方法:根据风险控制的原则,选择了人参种植实际使用农药、我国禁限用及高毒农药品种作为检测指标,共计192种。样品经乙腈超声提取浓缩后,在多反应监测模式(MRM)下进行检测,并采用分析保护剂-内标法定量以提高结果的准确性。其中对提取溶剂、净化方法[包括固相萃取法和快速样品前处理技术(Quechers)法]及色谱质谱条件都进行了考察和优化。结果:以人参为考察对象,本方法在1~100 μg·L-1线性良好,相关系数r>0.990,在5,20,100 μg·kg-1三水平进行加样回收率考察,98%的农药的平均回收率在70%~120%。11批样品中共检出14种农药单体,其中五氯硝基苯(PCNB)的检出率最高,按照2015年版《中国药典》人参、西洋参项下农残限度要求,不合格率达36%。结论:该方法检测指标针对性强,准确,快速,适用于人参中农药多残留的日常快速筛查。
Objective: To establish a method for simultaneous determination of 192 kinds of pesticide residues in ginseng by using gas and liquid chromatography tandem mass spectrometry (GC-MS/MS)
and determine 11 batches of ginseng samples(including Panacis Quinquefolii Radix
Ginseng Radix et Rhizoma
Ginseng Radix et Rhizoma Rubra and white ginseng). Method: The 192 types of pesticides commonly used in ginseng planting
forbidden in agriculture planting and those with high toxicity were selected as the detecting indexes in this method according to the risk control principals. The samples were extracted with acetonitrile
and the quantitative analysis was carried out by GC-MS/MS with multiple reaction monitoring (MRM) model. The analyte protectant-internal standard method was used to improve the accuracy of this method. The extraction solvents
purification methods (including solid phase extraction and Quechers)
and the conditions of chromatography-mass spectrometry were investigated and optimized. Result: The experimental results showed that the liner range for 192 pesticides were in the range of 1-100 μg·L-1 with correction coefficients of greater than 0.99.The average recoveries of 98% pesticides ranged from 70% to 120% at levels of 5
20
and 100 μg·kg-1. 14 kinds of pesticide monomers were detected in 11 batches of ginseng samples
and the detection rate of pentachloro-nitrobenzene(PCNB)was highest. According to the pesticide maximum residual limit(MRL)of ginseng and Panax quinquefolium in 2015 Chinese Pharmacopoeia
36% of the samples exceeded the MRL. Conclusion: This method has been proven accurate
quick
sensitive and suitable for determination of 192 pesticide residues in ginseng.
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