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Enantiomeric separation of malathion and malaoxon and the chiral residue analysis in food and environmental matrix.
Chirality ( IF 2 ) Pub Date : 2020-05-04 , DOI: 10.1002/chir.23229
Yifan Hua 1 , Qian Zhou 1 , Peng Wang 1 , Zhiqiang Zhou 1 , Donghui Liu 1
Affiliation  

Malathion is a widely used chiral phosphorus insecticide, which has a more toxic chiral metabolite malaoxon. In this work, the enantiomers of malathion and malaoxon were separated by high‐performance liquid chromatography‐mass/mass (HPLC‐MS/MS) with chiral columns using acetonitrile/water or methanol/water as mobile phase, and the chromatographic conditions were optimized. Based on the chiral separation, the chiral residue analysis methods for the enantiomers in soil, fruit, and vegetables were set up. Two pairs of the enantiomers were better separated on CHIRALPAK IC chiral column, and baseline simultaneous separations of malathion and malaoxon enantiomers were achieved with acetonitrile/water (40/60, v/v) as mobile phase at a flow rate of 0.5 mL/min. The elution orders were −/+ for both malathion and malaoxon measured by an optical rotation detector. The chiral residue analysis in soil, fruit, and vegetables was validated by linearity, recovery, precision, limit of detection (LOD), and limit of quantification (LOQ). The LODs and LOQs for the enantiomers of malathion were 1 μg/kg and 3–5 μg/kg and 0.08 μg/kg and 0.20–0.25 μg/kg for malaoxon enantiomers. Good linear calibration curves for each enantiomer in the matrices were obtained within the concentration range of 0.02–12 mg/L. The mean recoveries of the enantiomers of malathion and malaoxon ranged from 82.26% to 109.04%, with RSDs of 0.71–8.63%.The results confirmed that this method was capable of simultaneously determining the residue of malathion and malaoxon in food and environmental matrix on an enantiomeric level.

中文翻译:

食品和环境基质中马拉硫磷和马拉松的对映异构体分离以及手性残留物分析。

马拉硫磷是一种广泛使用的手性磷杀虫剂,它具有更强的手性代谢产物马拉oxon。在这项工作中,使用乙腈/水或甲醇/水作为流动相的高效液相色谱-质量/质量(HPLC-MS / MS)手性色谱柱分离了马拉硫磷和马拉松的对映体,并优化了色谱条件。基于手性分离,建立了土壤,水果和蔬菜中对映体的手性残留分析方法。在CHIRALPAK IC手性色谱柱上可以更好地分离两对对映异构体,并以乙腈/水(40/60,v / v)作为流动相,以0.5 mL / min的流速实现马拉硫磷和丙二酮对映体的基线同时分离。通过旋光检测器测得的马拉硫磷和马拉松的洗脱顺序为-/ +。通过线性,回收率,精密度,检测限(LOD)和定量限(LOQ)验证了土壤,水果和蔬菜中的手性残留物分析。马拉硫磷对映体的LOD和LOQ为1μg/ kg,3-5μg/ kg,0.08μg/ kg和0.20–0.25μg/ kg。在0.02-12 mg / L的浓度范围内,每种基质的对映体均具有良好的线性校准曲线。马拉硫磷和马拉松的对映体的平均回收率在82.26%至109.04%之间,相对标准偏差为0.71-8.63%。结果证实了该方法能够同时测定食品和环境基质中马拉硫磷和马拉松的残留量。对映体水平。通过线性,回收率,精密度,检测限(LOD)和定量限(LOQ)验证了土壤,水果和蔬菜中的手性残留物分析。马拉硫磷对映体的LOD和LOQ为1μg/ kg,3-5μg/ kg,0.08μg/ kg和0.20-0.25μg/ kg。在0.02-12 mg / L的浓度范围内,每种基质的对映体均具有良好的线性校准曲线。马拉硫磷和马拉松的对映体的平均回收率在82.26%至109.04%之间,相对标准偏差为0.71-8.63%。结果证实了该方法能够同时测定食品和环境基质中马拉硫磷和马拉松的残留量。对映体水平。通过线性,回收率,精密度,检测限(LOD)和定量限(LOQ)验证了土壤,水果和蔬菜中的手性残留物分析。马拉硫磷对映体的LOD和LOQ为1μg/ kg,3-5μg/ kg,0.08μg/ kg和0.20-0.25μg/ kg。在0.02-12 mg / L的浓度范围内,每种基质的对映体均具有良好的线性校准曲线。马拉硫磷和马拉松的对映体的平均回收率在82.26%至109.04%之间,相对标准偏差为0.71-8.63%。结果证实了该方法能够同时测定食品和环境基质中马拉硫磷和马拉松的残留量。对映体水平。和定量限(LOQ)。马拉硫磷对映体的LOD和LOQ为1μg/ kg,3-5μg/ kg,0.08μg/ kg和0.20–0.25μg/ kg。在0.02-12 mg / L的浓度范围内,每种基质的对映体均具有良好的线性校准曲线。马拉硫磷和马拉松的对映体的平均回收率在82.26%至109.04%之间,相对标准偏差为0.71-8.63%。结果证实了该方法能够同时测定食品和环境基质中马拉硫磷和马拉松的残留量。对映体水平。和定量限(LOQ)。马拉硫磷对映体的LOD和LOQ为1μg/ kg,3-5μg/ kg,0.08μg/ kg和0.20-0.25μg/ kg。在0.02-12 mg / L的浓度范围内,每种基质的对映体均具有良好的线性校准曲线。马拉硫磷和马拉松的对映体的平均回收率在82.26%至109.04%之间,相对标准偏差为0.71-8.63%。结果证实了该方法能够同时测定食品和环境基质中马拉硫磷和马拉松的残留量。对映体水平。在0.02-12 mg / L的浓度范围内,每种基质的对映体均具有良好的线性校准曲线。马拉硫磷和马拉松的对映体的平均回收率在82.26%至109.04%之间,相对标准偏差为0.71-8.63%。结果证实了该方法能够同时测定食品和环境基质中马拉硫磷和马拉松的残留量。对映体水平。在0.02-12 mg / L的浓度范围内,每种基质的对映体均具有良好的线性校准曲线。马拉硫磷和马拉松的对映体的平均回收率在82.26%至109.04%之间,相对标准偏差为0.71-8.63%。结果证实了该方法能够同时测定食品和环境基质中马拉硫磷和马拉松的残留量。对映体水平。
更新日期:2020-05-04
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