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Fast determination of phenoxy acid herbicides in carrots and apples using liquid chromatography coupled triple quadrupole mass spectrometry

机译:液相色谱-三重四极杆质谱联用法快速测定胡萝卜和苹果中的苯氧基酸除草剂

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摘要

A fast, simple and inexpensive method has been developed for the analysis of phenoxy acid herbicides: 2,4-dichloropheno-xyacetic acid (2,4-D), 4-chloro-2-methylphenoxyacetic acid (MCPA), 2-(4-chloro-o-tolyloxy)propionic acid (MCPP), 2-(4-aryloxyphenoxy)propionic acid (Fluazifop) and 2-(4-aryloxyphenoxy)propionic acid (Haloxyfop) in carrots and apples by liquid chromatography coupled to triple quadrupole mass spectrometry (LC/MS/MS). The compounds were analyzed by QuEChERS (quick, easy, cheap, effective, rugged, safe) methodology without cleanup.rnThe recoveries were performed at two spiked levels (0.05 and 0.5 mg/kg) for both matrices with six replicates for each level. The mean recoveries ranged from 70-92% for both apples and carrots. The precision of the method expressed as relative standard deviation (RSD%) was found to be in the range 3-15%. For all compounds, good linearity (r~2 > 0.99) was obtained over the range of concentration from 0.05 μg/mL to 0.5 μg/mL, corresponding to the pesticide concentrations of 0.05 mg/kg and 0.5 mg/kg, respectively. The determination limits (LOQs) ranged from 0.01 ng/mL to 1.3 ng/mL in solvent, whereas, the LOQs calculated in matrix ranged from 0.05 ng/g to 21.0 ng/g for apples and from 0.06 ng/g to 10.2 ng/g for carrots. The developed methodology combines the advantages of both QuEChERS and LC/MS/MS producing a very rapid, sensitive and cheap method useful for the routine analytical laboratories.
机译:已经开发了一种快速,简单且廉价的方法来分析苯氧基酸除草剂:2,4-二氯苯氧乙酸(2,4-D),4-氯-2-甲基苯氧乙酸(MCPA),2-(4液相色谱法联用三重四极杆质谱联用分析胡萝卜和苹果中的-氯-邻甲苯甲氧基)丙酸(MCPP),2-(4-芳氧基苯氧基)丙酸(Fluazifop)和2-(4-芳氧基苯氧基)丙酸(Haloxyfop)光谱法(LC / MS / MS)。通过QuEChERS(快速,简便,便宜,有效,坚固,安全)方法对化合物进行分析,无需纯化。两种基质的回收率均以两个加标水平(0.05和0.5 mg / kg)进行,每个水平重复六次。苹果和胡萝卜的平均回收率在70-92%之间。发现以相对标准偏差(RSD%)表示的方法精度在3-15%的范围内。对于所有化合物,在0.05μg/ mL至0.5μg/ mL的浓度范围内均获得了良好的线性(r〜2> 0.99),分别对应于农药浓度0.05 mg / kg和0.5 mg / kg。溶剂中的测定限(LOQs)在0.01 ng / mL至1.3 ng / mL之间,而矩阵中计算的LOQ在苹果中则在0.05 ng / g至21.0 ng / g之间,在0.06 ng / g至10.2 ng / g之间。 g代表胡萝卜。所开发的方法结合了QuEChERS和LC / MS / MS的优点,可提供一种非常快速,灵敏且廉价的方法,可用于常规分析实验室。

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