摘要
目的通过气相色谱-串联质谱(GC-MS/MS)技术建立测定山药中联苯菊酯等3种农药残留的一测多评方法。方法样品采用乙腈提取,经Cleanert TPH专用净化柱净化。根据色谱相对保留时间和质荷比信息对样品进行定性分析,以联苯菊酯二级离子扫描(母离子与子离子的质荷比之比为181.1/166.1)峰面积为参照,并建立以联苯菊酯为对照品,测定山药中联苯菊酯等3种农药残留量的GC-MS/MS方法。结果联苯菊酯、甲氰菊酯、溴氰菊酯进样量在0.01~0.10 ng范围内均与自身色谱峰面积线性关系较好,最低检出限(以进样量计)依次为7.684×10^(-5) ng,1.021×10^(-4) ng和2.177×10^(-3) ng,平均回收率依次为93.66%,93.11%和92.95%,RSD依次为0.81%,0.55%和0.69%(n=9)。结论该一测多评方法简单、快速、定量准确,适用于山药中农药残留的测定。
Objective To establish a quantitative analysis of multi-components by single marker（ QAMS） method for the determination of 3 pesticide residues such as bifenthrin in Rhizoma Dioscoreae by GC-MS/MS. Methods The samples were extracted by acetonitrile and purified by Cleanert TPH column. Information on relative retention time（ RRT） and mass-to-charge ratio was used for qualitative analysis. The peak area of secondary ion MS of bifenthrin（ 181. 1/166. 1） was used as the reference to establish a method of using bifenthrin as the reference substance to determinate 3 pesticide residues in Rhizoma Dioscoreae by GC-MS/MS. Results The sample size of bifenthrin,fenpropathrin and deltamethrin in the range of 0. 01-0. 10 ng has good linear relationships with the peak area of its own chromatography. Limit of quantification（ LOQ） of bifenthrin,fenpropathrin and deltamethyrin were 7. 684 × 10^（-5） ng,1. 021 × 10^（-4） ng and 2. 177 × 10^（-3） ng,respectively. The average recovery rates of bifenthrin,fenpropathrin and deltamethyrin were 93. 66%,93. 11% and92. 95%,respectively,RSDs were 0. 81%,0. 55% and 0. 69%（ n = 9）. Conclusion The QAMS method is simple,quick,quantitative and accurate,which is suitable for the determination of pesticide residues in Rhizoma Dioscoreae.
出处
《中国药业》
CAS
2018年第2期30-34,共5页
China Pharmaceuticals
关键词
气相色谱-串联质谱法
山药
联苯菊酯
甲氰菊酯
溴氰菊酯
含量测定
农药残留
一测多评
GC - MS/MS
Rhizoma Dioscoreae
bifenthrin
fenpropathrin
deltamethyrin
content determination
pesticide residues
quantitative analysis of multi - components by single marker
