QuEChERS-液相色譜-串聯質譜法測定植物源食品中氟噻草胺和乙酰甲草胺殘留
發(fā)布時間：2019-03-27 15:59
【摘要】：建立了QuEChERS前處理-液相色譜-串聯質譜儀(HPLC-MS/MS)測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,提取液經離心、過膜后直接上機檢測。該方法采用C18色譜柱進行色譜分離,以0.1%甲酸水(含5mmol/mL乙酸銨)-甲醇為流動相,在0.25mL/min流速下梯度洗脫,電噴霧正離子電離(ESI+),多重反應監(jiān)測模式(MRM)檢測,以保留時間和特征離子對(母離子和兩個碎片離子)信息比較進行定性,基質匹配曲線定量。在9種基質(葡萄、葡萄干、黃瓜、小麥粉、蘋果、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范圍內線性關系良好,相關系數均大于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個添加水平下,氟噻草胺的平均回收率在82.5%~103.9%,相對標準偏差為2.9%~15%;乙酰甲草胺的回收率在81.7%~108.1%,相對標準偏差在3.1%~14%。方法靈敏度、準確度和精密度均符合農藥殘留檢測要求。
[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】： 中國檢驗檢疫科學研究院食品安全研究所;伊犁出入境檢驗檢疫局綜合技術服務中心;溫州出入境檢驗檢疫局;
【分類號】：O657.63
本文編號：2448334
[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】： 中國檢驗檢疫科學研究院食品安全研究所;伊犁出入境檢驗檢疫局綜合技術服務中心;溫州出入境檢驗檢疫局;
【分類號】：O657.63
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