摘要
实验建立了同时测定白术中498种农药残留量的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法,并对不同产地的30批白术药材进行测定。样品经1%冰醋酸乙腈提取,加入无水硫酸镁、N-丙基乙二胺(PSA)、十八烷基硅烷键合硅胶、硅胶和石墨化炭黑(GCB)进行分散固相萃取净化,采用HPLC-MS/MS分析,内标法定量。结果显示498个农药成分在5~400 ng·mL^(-1)有良好的线性关系,相关系数r>0.990。在线性范围内,498个农药成分在3个添加水平(加标水平:0.05、0.10、0.20 mg·kg(-1)下,除杀草隆、灭螨猛、甲氨基阿维菌素苯甲酸盐外,其余495种农药加样回收率在61.18%~132.1%,RSD在0.24%~15%。30批样品中共检出16种农药成分。其中苯醚甲环唑、戊唑醇检出率较高,苯醚甲环唑检出率为76.7%,4个批次的样品残留量超出《中国药典》规定的33种禁用农药定量限,除禁用农药外的农药组分使用理论最大残留限量作为安全风险判断标准,噻虫胺、苯醚甲环唑、甲基嘧啶磷的检出超出理论最大残留限量。该文建立的方法易于操作,结果可靠,可用于白术中农药残留的定性和定量分析。
A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was established for the simultaneous determination of 498 farm chemical residues in Atractylodis Macrocephalae Rhizoma.Furthermore,the established method was used to determine the residues in 30 batches of Atractylodis Macrocephalae Rhizoma samples from different habitats.The samples were extracted with acetonitrile containing 1%glacial acetic acid,and the extract was purified by dispersive solid-phase extraction with sorbents of magnesium sulfate,primary secondary amine(PSA),C_(18),silica gel,and graphitized carbon black(GCB).The prepared samples were then analyzed by HPLC-MS/MS,and the internal standard method was used to quantify the residues.The experimental results showed that the 498 farm chemicals presented good linear relationship within the range of 5-400 ng·mL^(-1),with correction coefficients greater than 0.990.Within the linear ranges,the recovery of 495 farm chemicals(except daimuron,chinomethionat,and emamectin benzoate)at three spiked levels(0.05,0.10,and 0.20 mg·kg^(-1))was in the range of 61.18%-132.1%,with the RSD of 0.24%-15%.A total of 16 farm chemicals were detected in 30 batches of samples.Among them,difenoconazole and tebuconazole showed higher detection rates,and the detection rate of difenoconazole was 76.7%.The residues of 4 batches of samples exceeded the limits of quantitation of 33 banned farm chemicals stipulated in the Chinese Pharmacopoeia.The theoretical maximum residue limits of the farm chemicals except banned farm cheimicals were used as the judgment standard of safety risks,under which the detected residues of clothianidin,difenoconazole,and pirimiphos-methyl exceeded the theoretical maximum residue limits.The new method established in this paper is simple and reliable,and it can thus be used for qualitative and quantitative analyses of farm chemical residues in Atractylodis Macrocephalae Rhizoma.
作者
陈白雪
吴玉强
白桂昌
罗轶
CHEN Bai-xue;WU Yu-qiang;BAI Gui-chang;LUO Yi(Guangxi University of Chinese Medicine,Nanning 530001,China;Guangxi University of Chinese Medicine Bainianle Pharmaceutical Co.,Ltd.,Nanning 530023,China;Guangxi Institute for Drug Control,Nanning 530021,China)
出处
《中国中药杂志》
北大核心
2025年第8期2090-2107,共18页
China Journal of Chinese Materia Medica
基金
国家药典委员会2022年度国家药品标准制修订研究项目(2022Z02)。
作者简介
陈白雪,硕士研究生,研究方向为中药制剂研究与开发,E-mail:chenbaixue2022@stu.gxtcmu.edu.cn;通信作者:吴玉强,硕士,教授级高级工程师,研究方向为中药成分分析与质量控制,E-mail:409444015@qq.com;通信作者:白桂昌,学士,主管药师,研究方向为中药质量与安全,E-mail:353246271@qq.com。
