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气相色谱-质谱联用同时测定猕猴桃中农药残留的不同提取方法比较

Comparison of different extraction methods for the simultaneous determination of pesticide residues in kiwi fruit using gas chromatography-mass spectrometry.

作者信息

Cho Soon-Kil, Abd El-Aty A M, Jeon Hyang-Rang, Choi Jeong-Heui, Shin Ho-Chul, Shim Jae-Han

机构信息

Natural Products Chemistry Laboratory, Institute of Agricultural Science and Technology, College of Agriculture and Life Science, Chonnam National University, 300 Yong-Bong Dong, Buk-Ku, Gwangju 500-757, Republic of Korea.

出版信息

Biomed Chromatogr. 2008 Jul;22(7):727-35. doi: 10.1002/bmc.990.

Abstract

The methods of simultaneous extraction of iprodione, chlorpyrifos-methyl, EPN and endosulfan (with its metabolites) from kiwi fruit using accelerated solvent extraction (ASE), supercritical fluid extraction (SFE), and liquid-liquid extraction (LLE) were tested and compared in terms of their of limits of detection and quantification, as well as the highest pesticide recoveries with the lowest residues in the final extracts. The analysis was performed using gas chromatography-mass spectrometry in the selected ion monitoring mode. The proposed methods featured good sensitivity, pesticide quantification limits were low enough, and the precision (expressed as relative standard deviations) ranged from 0.56 to 7.17%. The recoveries obtained from ASE, SFE and LLE were 77.5-120, 71.9-109.1 and 75.6-127.1%, respectively. The proposed methods were successfully applied for the monitoring of the selected pesticide residues in kiwi fruit samples collected from Jollanamdo area, Republic of Korea. Iprodione was detected at a level lower than the maximum residue limit (MRL) established by the Korea Food and Drug Administration (5 ppm), while EPN was detected at a level higher than the Korea Food and Drug Administration MRL (0.1 ppm) in the real samples. The proposed sample preparations led to a higher preconcentration of the pesticide fraction, and allowed the sensitive and selective determination of pesticides with varied physicochemical properties in kiwi fruit.

摘要

采用加速溶剂萃取(ASE)、超临界流体萃取(SFE)和液液萃取(LLE)从猕猴桃中同时提取异菌脲、甲基毒死蜱、EPN和硫丹(及其代谢物)的方法,在检测限和定量限、最终提取物中农药残留量最低时的最高回收率方面进行了测试和比较。分析采用气相色谱 - 质谱联用的选择离子监测模式进行。所提出的方法具有良好的灵敏度,农药定量限足够低,精密度(以相对标准偏差表示)范围为0.56%至7.17%。ASE、SFE和LLE的回收率分别为77.5 - 120%、71.9 - 109.1%和75.6 - 127.1%。所提出的方法成功应用于监测从韩国全罗南道地区采集的猕猴桃样品中选定的农药残留。在实际样品中,异菌脲的检测水平低于韩国食品药品管理局规定的最大残留限量(MRL,5 ppm),而EPN的检测水平高于韩国食品药品管理局的MRL(0.1 ppm)。所提出的样品制备方法使农药组分得到更高的预浓缩,并能够灵敏且选择性地测定猕猴桃中具有不同理化性质的农药。

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