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超高效液相色谱–串联质谱法检测果蔬中的吡氟甲禾灵残留
引用本文:武婷,段迎燕,田海娇. 超高效液相色谱–串联质谱法检测果蔬中的吡氟甲禾灵残留[J]. 化学分析计量, 2016, 0(5): 68-71. DOI: 10.3969/j.issn.1008-6145.2016.05.018
作者姓名:武婷  段迎燕  田海娇
作者单位:山西省分析科学研究院,太原,030006
摘    要:建立了超高效液相色谱–串联质谱(UPLC–MS/MS)法测定果蔬中吡氟甲禾灵残留的方法。样品以乙腈匀浆提取,并采用Sep-Pak Vac型氨基固相萃取柱净化样品,采用超高效液相色谱柱WATERS ACQUITY C_(18)柱(50mm×2.1 mm,1.7μm)分离,以乙腈–0.1%甲酸水溶液作为淋洗液进行梯度洗脱。吡氟甲禾灵在1.0~50.0 ng/m L范围内线性关系良好,相关系数r~2=0.997 7,加标回收率为84.1%~88.6%,测定结果的相对标准偏差为1.18%~3.58%(n=6)。该方法操作简便,分析快速,提取效率高,重现性好,有实用价值。

关 键 词:超高效液相色谱-质谱法  果蔬  吡氟甲禾灵

Determination of Haloxyfop-methyl Residue in Fruits and Vegetables by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry
Abstract:A method for determination of haloxyfop-methyl residue in fruits and vegetables was developed by using ultra high performance liquid chromatography–tandem mass spectrometry(UPLC–MS/MS). The samples were extracted by acetonitrile firstly and the extracts were cleaned using Sep-Pak Vac-SPE column, the extracts were then separated by a WATERS ACQUITY C18 column (50 mm×2.1 mm,1.7μm) utilizing gradient elution with acetonitrile–0.1% formic acid. The linear relationship was fine in the concentration range of 1.0–50.0 ng/mL withr2 of 0.997 7, the recoveries were in the range of 84.1%–88.6%,RSDs were in the range of 1.18%–3.58%(n=6). The method has the advantage of simple operation, rapid analysis, high extraction efficiency, good reproducibility and practical value.
Keywords:ultra high performance liquid chromatography-mass spectrometry  fruits and vegetables  haloxyfop-methyl
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