發(fā)布時(shí)間：2019-03-27 15:59

【摘要】：建立了QuEChERS前處理-液相色譜-串聯(lián)質(zhì)譜儀(HPLC-MS/MS)測(cè)定植物源食品中氟噻草胺和乙酰甲草胺殘留量的分析方法。樣品經(jīng)酸化乙腈(含0.1%甲酸的乙腈)提取,采用石墨化碳黑(GCB)凈化,提取液經(jīng)離心、過(guò)膜后直接上機(jī)檢測(cè)。該方法采用C18色譜柱進(jìn)行色譜分離,以0.1%甲酸水(含5mmol/mL乙酸銨)-甲醇為流動(dòng)相,在0.25mL/min流速下梯度洗脫,電噴霧正離子電離(ESI+),多重反應(yīng)監(jiān)測(cè)模式(MRM)檢測(cè),以保留時(shí)間和特征離子對(duì)(母離子和兩個(gè)碎片離子)信息比較進(jìn)行定性,基質(zhì)匹配曲線定量。在9種基質(zhì)(葡萄、葡萄干、黃瓜、小麥粉、蘋(píng)果、白菜、枸杞、西紅柿和大米)中,氟噻草胺和乙酰甲草胺在0.25~25.0μg/L范圍內(nèi)線性關(guān)系良好,相關(guān)系數(shù)均大于0.997,兩種化合物的方法定量限為0.5μg/kg;在0.5,1.0,5.0μg/kg3個(gè)添加水平下,氟噻草胺的平均回收率在82.5%~103.9%,相對(duì)標(biāo)準(zhǔn)偏差為2.9%~15%;乙酰甲草胺的回收率在81.7%~108.1%,相對(duì)標(biāo)準(zhǔn)偏差在3.1%~14%。方法靈敏度、準(zhǔn)確度和精密度均符合農(nóng)藥殘留檢測(cè)要求。
[Abstract]:A QuEChERS pretreatment-liquid chromatography-tandem mass spectrometer (HPLC-MS/MS) method for the determination of fluorothiochlor and acetylalachlor residues in vegetable foods was established. The sample was extracted with acidified acetonitrile (acetonitrile containing 0.1% formic acid) and purified by graphitized carbon black (GCB). The chromatographic separation was carried out on C18 column, 0.1% formic acid water (containing 5mmol/mL ammonium acetate)-methanol as mobile phase, gradient elution at 0.25mL/min flow rate, electrospray ionization of (ESI),. Multiple reaction monitoring mode (MRM) detection was used to compare the retention time and the information of characteristic ion pairs (parent ion and two fragment ions), and the matrix matching curve was quantified. In 9 substrates (grapes, raisins, cucumbers, wheat flour, apples, cabbage, Lycium barbarum, tomatoes and rice), there was a good linear relationship between fluothiochlor and acetylalachlor in the range of 0.25 ~ 25.0 渭 g / L, and the correlation coefficients were more than 0.997, The quantitative limit of the two compounds is 0.5 渭 g / kg;. At 0.5, 1.0,5.0 渭 g / kg3, the average recovery was 82.5% ~ 103.9%, and the relative standard deviation (RSD) was 2.9% ~ 15%. The recovery of Acetochlor was 81.7% ~ 108.1%, and the relative standard deviation (RSD) was 3.1% ~ 14%. The sensitivity, accuracy and precision of the method meet the requirements of pesticide residue detection.
【作者單位】： 中國(guó)檢驗(yàn)檢疫科學(xué)研究院食品安全研究所;伊犁出入境檢驗(yàn)檢疫局綜合技術(shù)服務(wù)中心;溫州出入境檢驗(yàn)檢疫局;
【分類號(hào)】：O657.63

【相似文獻(xiàn)】

相關(guān)會(huì)議論文 前1條

1 章晴;陳士恒;楊永壇;王福榮;;QuEChERS-氣相色譜法測(cè)定綠茶中有機(jī)磷類農(nóng)藥殘留[A];全國(guó)生物醫(yī)藥色譜及相關(guān)技術(shù)學(xué)術(shù)交流會(huì)（2012）會(huì)議手冊(cè)[C];2012年

相關(guān)碩士學(xué)位論文 前1條

1 莊奕筠;中樞神經(jīng)系統(tǒng)藥物的QuEChERS-液質(zhì)聯(lián)用系統(tǒng)分析[D];福建醫(yī)科大學(xué);2015年

，

本文編號(hào)：2448334