【摘要】：建立了蔬菜和水果中雙三氟蟲脲、四氯蟲酰胺和氰蟲酰胺3種新型殺蟲劑的分散固相萃取-液相色譜-串聯(lián)質(zhì)譜檢測(cè)方法。樣品經(jīng)乙腈均質(zhì)提取,混合使用乙二胺-N-丙基硅烷(PSA)和C18基質(zhì)分散凈化劑進(jìn)行凈化,液相色譜-三重四極桿串聯(lián)質(zhì)譜(LC-MS/MS)同時(shí)進(jìn)行檢測(cè)。雙三氟蟲脲和四氯蟲酰胺采用多反應(yīng)監(jiān)測(cè)負(fù)離子模式,氰蟲酰胺采用多反應(yīng)監(jiān)測(cè)正離子模式。雙三氟蟲脲在蘋果、洋蔥和經(jīng)微波處理的洋蔥樣品中均不存在基質(zhì)效應(yīng),可采用純?nèi)軇?biāo)準(zhǔn)外標(biāo)法或者采用基質(zhì)匹配標(biāo)準(zhǔn)溶液定量檢測(cè);四氯蟲酰胺和氰蟲酰胺存在程度不同的基質(zhì)減弱效應(yīng),采用空白基質(zhì)匹配的校正標(biāo)準(zhǔn)曲線外標(biāo)法定量。3種殺蟲劑均在0.2~100μg/L線性范圍內(nèi)具有良好的線性關(guān)系,相關(guān)系數(shù)均大于0.9990。在0.005~2.000 mg/kg范圍內(nèi),平均添加回收率為81.6%~99.9%,相對(duì)標(biāo)準(zhǔn)偏差為3.6%~9.8%。氰蟲酰胺、四氯蟲酰胺和雙三氟蟲脲的檢出限分別為0.064,0.048和0.001μg/kg,定量限分別為0.210,0.160和0.004μg/kg。
[Abstract]:A method for the determination of three new insecticides in vegetables and fruits by dispersive solid-phase extraction-liquid chromatography-tandem mass spectrometry was developed. The samples were extracted by acetonitrile homogenization and purified by ethylenediamine-N-propylsilane (PSA) and C18 matrix dispersion purifier. The samples were detected by liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS). The negative ion pattern was monitored by multi-reaction and the positive ion pattern was monitored by multi-reaction of dichloromide and tetrachloromide. There was no matrix effect in apple, onion and microwave treated onion samples, which could be detected by standard external standard method of pure solvent or matrix matching standard solution. The matrix weakening effect of tetrachloromide and cyanamide was different. The calibration standard curve external standard method for blank matrix matching was used to quantify the three insecticides. There was a good linear relationship in the linear range of 0.2 渭 g / L for all three insecticides. The correlation coefficient is more than 0.9990. In the range of 0.005 ~ 2.000 mg/kg, the average recovery was 81.6 ~ 99.9 and the relative standard deviation was 3.6 ~ 9.8. The detection limits of cyandiamide, tetrachloromide and dichloromide were 0.064 渭 g / kg and 0.001 渭 g / kg, respectively, and the quantification limits were 0.210 渭 g / kg and 0.004 渭 g / kg, respectively.
【作者單位】： 山東出入境檢驗(yàn)檢疫局檢驗(yàn)檢疫技術(shù)中心;山東省農(nóng)業(yè)科學(xué)院植物保護(hù)研究所;
【基金】：山東出入境檢驗(yàn)檢疫科研項(xiàng)目(No.SK201425)資助
【分類號(hào)】：TS255.7;O657.63

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