本文選題：中藥　切入點(diǎn)：農(nóng)藥多殘留　出處：《中國(guó)藥學(xué)雜志》2016年05期

【摘要】：目的以金銀花、枸杞子為代表性基質(zhì),建立了花和果實(shí)類中藥材中187種農(nóng)藥多殘留的氣相色譜-串聯(lián)質(zhì)譜(GC-MS/MS)及液相色譜-串聯(lián)質(zhì)譜(LC-MS/MS)檢測(cè)方法,并應(yīng)用于8種藥材50余批次樣品初步篩查。方法依據(jù)風(fēng)險(xiǎn)控制的基本原則選擇我國(guó)禁限用、高毒高風(fēng)險(xiǎn)及常用農(nóng)藥品種作為檢測(cè)指標(biāo)。實(shí)驗(yàn)過(guò)程中對(duì)提取溶劑、凈化條件及色譜質(zhì)譜條件都進(jìn)行了探索和優(yōu)化。最終方法經(jīng)乙腈超聲提取,石墨炭黑固相萃取柱凈化,分別以氣相和液相色譜分離,在串聯(lián)質(zhì)譜多反應(yīng)監(jiān)測(cè)模式(MRM)下進(jìn)行測(cè)定。GC-MS/MS和LC-MS/MS皆采用內(nèi)標(biāo)法計(jì)算以提高結(jié)果的準(zhǔn)確性。結(jié)果以金銀花、枸杞子作為考察對(duì)象,本方法在1~100 ng·m L~(-1)之間線性良好,相關(guān)系數(shù)r0.990 0;在質(zhì)量比為5、20、100μg·kg~(-1)的三水平加標(biāo)回收實(shí)驗(yàn)中,88%以上的農(nóng)藥平均回收率在70%~120%之間。結(jié)論該方法檢測(cè)指標(biāo)針對(duì)性強(qiáng),涵蓋大部分中草藥中的禁限用農(nóng)藥,檢測(cè)方法快速、準(zhǔn)確,適用于花類、果實(shí)類中藥中農(nóng)藥殘留的日常檢測(cè)。
[Abstract]:Objective to establish gas chromatography-tandem mass spectrometry (GC-MS / MS) and liquid chromatography-tandem mass spectrometry (LC-MS / MS) methods for the determination of 187 pesticide residues in Flos Lonicerae (Flos Lonicerae) and Fructus Lycii (Fructus Lycii). It was applied to the preliminary screening of more than 50 batches of 8 kinds of medicinal materials. Methods according to the basic principles of risk control, the banned, highly toxic and common pesticide varieties in China were selected as the detection indexes. The extraction solvent was used in the process of the experiment. The purification conditions and chromatography-mass spectrometry conditions were explored and optimized. The final method was extracted by acetonitrile and purified by solid phase extraction column with graphite carbon black, and separated by gas and liquid chromatography, respectively. Both GC-MS / MS and LC-MS/MS were calculated by internal standard method to improve the accuracy of the results. Results the method was linear with honeysuckle and wolfberry. The linear range of this method was 1100ng / mL ~ (-1). The average recovery rate of above 88% was between 70% and 120% in the three-level standard recovery experiment with a mass ratio of 5 ~ 20100 渭 g 路kg ~ (-1) ~ (-1). Conclusion the detection index of this method has strong pertinence and covers the banned pesticides in most Chinese herbal medicines, and the detection method is rapid. Accurate, suitable for the daily detection of pesticide residues in flowers and fruits.
【作者單位】： 中國(guó)食品藥品檢定研究院;
【基金】：國(guó)家十二五“重大新藥創(chuàng)制”專項(xiàng)資助項(xiàng)目(2014ZX09304307-002)
【分類號(hào)】：R284.1;O657.63
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本文編號(hào)：1652943