發(fā)布時(shí)間：2018-02-04 11:12

  本文關(guān)鍵詞： 液相色譜-串聯(lián)質(zhì)譜 蜂蜜 蜂花粉 吡蟲啉 吡蟲啉烯烴 吡蟲啉脲 -氯煙酸 增強(qiáng)型脂類去除材料　出處：《分析化學(xué)》2017年04期 　論文類型：期刊論文

【摘要】：建立了蜂蜜和蜂花粉中吡蟲啉及其代謝物吡蟲啉烯烴、吡蟲啉脲、6-氯煙酸的液相色譜-串聯(lián)質(zhì)譜(LC-MS/MS)檢測(cè)方法。在Qu ECh ERS方法基礎(chǔ)上,針對(duì)目標(biāo)物化學(xué)性質(zhì)和樣品雜質(zhì)情況,對(duì)提取溶液的p H值、提取次數(shù)、凈化材料等參數(shù)進(jìn)行了優(yōu)化。最終以5%甲酸-乙腈溶液提取兩次,無(wú)水Mg SO_4、NaCl鹽析分層,提取液經(jīng)增強(qiáng)型脂類去除材料(EMR)凈化,以LC-MS/MS進(jìn)行測(cè)定,基質(zhì)外標(biāo)法進(jìn)行定量分析。結(jié)果表明,蜂蜜和蜂花粉中吡蟲啉、吡蟲啉烯烴、吡蟲啉脲、6-氯煙酸的平均加標(biāo)回收率為86.0%~111.5%,相對(duì)標(biāo)準(zhǔn)偏差在1.7%~9.6%之間,檢出限分別為0.20、3.50、0.40和14.00μg/kg,定量限分別為0.60、11.64、1.20和45.00μg/kg。本方法分析速度快、靈敏度高、重現(xiàn)性好,適用于蜂蜜和蜂花粉中吡蟲啉及其3種代謝物的快速測(cè)定。
[Abstract]:Imidacloprid and its metabolite imidacloprid olefin and imidacloprid urea in honey and bee pollen were established. Determination of 6-Chlorotinic Acid by liquid Chromatography-tandem Mass Spectrometry (LC-MS / MS). Based on the qu ECh ERS method, the chemical properties of the target and the impurity of the sample were studied. The pH value of extraction solution, extraction times and purification materials were optimized. Finally, 5% formic acid-acetonitrile solution was used to extract twice, and anhydrous mg so _ 4 + NaCl salting out was stratified. The extract was purified by enhanced lipids removal material (EMR), determined by LC-MS/MS and quantitatively analyzed by matrix external standard method. The results showed that imidacloprid and imidacloprid olefins were found in honey and bee pollen. The average recovery of imidacloprid 6-chlorniacin was 86.0 and 111.5, the relative standard deviation was between 1.7 and 9.6%, and the detection limit was 0.20 ~ 3.50. The quantitative limits of 0.40 渭 g / kg and 14.00 渭 g / kg were 0.60 渭 g / kg and 45.00 渭 g / kg, respectively. It is suitable for rapid determination of imidacloprid and its three metabolites in honey and bee pollen.
【作者單位】： 省部共建國(guó)家重點(diǎn)實(shí)驗(yàn)室培育基地"浙江省植物有害生物防控重點(diǎn)實(shí)驗(yàn)室"農(nóng)業(yè)部農(nóng)藥殘留檢測(cè)重點(diǎn)實(shí)驗(yàn)室浙江省農(nóng)業(yè)科學(xué)院農(nóng)產(chǎn)品質(zhì)量標(biāo)準(zhǔn)研究所;南京農(nóng)業(yè)大學(xué)植物保護(hù)學(xué)院;中國(guó)農(nóng)業(yè)大學(xué)理學(xué)院;中國(guó)農(nóng)業(yè)科學(xué)院蜜蜂研究所;
【基金】：浙江省自然基金項(xiàng)目(No.LQ14B070004) 特色農(nóng)產(chǎn)品全產(chǎn)業(yè)鏈安全風(fēng)險(xiǎn)管控項(xiàng)目(No.ZJNY2016001) 蜂產(chǎn)品全產(chǎn)業(yè)鏈安全風(fēng)險(xiǎn)管控項(xiàng)目(No.ZJNY2016001-02)資助
【分類號(hào)】：S896.8;O657.63
【正文快照】： 1引言新煙堿類殺蟲劑為昆蟲乙酰膽堿受體激動(dòng)劑,是繼有機(jī)磷類、氨基甲酸酯類和擬除蟲菊酯類等殺蟲劑之后的第四大類殺蟲劑[1]。吡蟲啉是其代表性藥劑,主要用于防治水稻、小麥、棉田中的蚜蟲、葉蟬、飛虱等30多種刺吸式口器害蟲、地下害蟲[2]。吡蟲啉對(duì)哺乳動(dòng)物低毒,但對(duì)蜜蜂具，

本文編號(hào)：1490069