QuEChERS-液相色谱-串联质谱法测定植物源食品中氟噻草胺和乙酰甲草胺残留
发布时间：2019-03-27 15:59
【摘要】：建立了QuEChERS前处理-液相色谱-串联质谱仪(HPLC-MS/MS)测定植物源食品中氟噻草胺和乙酰甲草胺残留量的分析方法。样品经酸化乙腈(含0.1%甲酸的乙腈)提取,采用石墨化碳黑(GCB)净化,提取液经离心、过膜后直接上机检测。该方法采用C18色谱柱进行色谱分离,以0.1%甲酸水(含5mmol/mL乙酸铵)-甲醇为流动相,在0.25mL/min流速下梯度洗脱,电喷雾正离子电离(ESI+),多重反应监测模式(MRM)检测,以保留时间和特征离子对(母离子和两个碎片离子)信息比较进行定性,基质匹配曲线定量。在9种基质(葡萄、葡萄干、黄瓜、小麦粉、苹果、白菜、枸杞、西红柿和大米)中,氟噻草胺和乙酰甲草胺在0.25~25.0μg/L范围内线性关系良好,相关系数均大于0.997,两种化合物的方法定量限为0.5μg/kg;在0.5,1.0,5.0μg/kg3个添加水平下,氟噻草胺的平均回收率在82.5%~103.9%,相对标准偏差为2.9%~15%;乙酰甲草胺的回收率在81.7%~108.1%,相对标准偏差在3.1%~14%。方法灵敏度、准确度和精密度均符合农药残留检测要求。
[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.
【作者单位】： 中国检验检疫科学研究院食品安全研究所;伊犁出入境检验检疫局综合技术服务中心;温州出入境检验检疫局;
【分类号】：O657.63
本文编号：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.
【作者单位】： 中国检验检疫科学研究院食品安全研究所;伊犁出入境检验检疫局综合技术服务中心;温州出入境检验检疫局;
【分类号】：O657.63
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