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超临界流体色谱法快速测定果蔬泥中拟除虫菊酯fenpropathrin 对映体的研究方法。

Research method of rapid determination of chiral pesticide fenpropathrin enantiomers in fruit and vegetable puree by supercritical fluid chromatography.

机构信息

Zhejiang Academy of Science and Technology for Inspection and Quarantine, Hangzhou, P. R. China.

Technical Center of Xiamen Customs, Xiamen, P. R. China.

出版信息

J Sep Sci. 2022 Jul;45(14):2717-2723. doi: 10.1002/jssc.202200147. Epub 2022 May 18.

DOI:10.1002/jssc.202200147
PMID:35524724
Abstract

A method is first established for the separation and determination of fenpropathrin enantiomer residues in apple puree, strawberry puree, and tomato puree considered a supplementary food for infants by supercritical fluid chromatography. After the sample was extracted with acetonitrile and cleaned up by a solid-phase extraction column, then it was separated by a CHIRALPAK AD-3 chiral column with gradient elution at a flow rate of 1.5 mL/min using methanol and supercritical carbon dioxide as the mobile phase, detected by ultraviolet detector at 230 nm wavelength and quantified with the external standard method. The limits of quantification of the two fenpropathrin enantiomers were both 0.2 mg/kg, the linear ranges were 1.0-20.0 mg/L with linear correlation coefficients greater than 0.9992, the recoveries in the spiked samples at 0.2, 0.4 and 2.0 mg/kg were from 80.6 to 105%, and the relative standard deviation reached 2.6-7.7%. This method has the advantages of convenient operation, good resolution, and environmental protection, which can satisfy the requirement of determination for fenpropathrin enantiomer residues in fruit and vegetable puree as supplementary food for infants.

摘要

首先建立了一种超临界流体色谱法用于分离和测定婴幼儿补充食品苹果泥、草莓泥和番茄泥中顺式-氯氰菊酯对映体残留的方法。样品用乙腈提取,用固相萃取柱净化,然后以甲醇和超临界二氧化碳为流动相,在 1.5ml/min 的流速下用 CHIRALPAK AD-3 手性柱进行梯度洗脱,在 230nm 波长下用紫外检测器检测,并用外标法定量。两种顺式-氯氰菊酯对映体的定量限均为 0.2mg/kg,线性范围为 1.0-20.0mg/L,线性相关系数均大于 0.9992,在 0.2、0.4 和 2.0mg/kg 添加水平下的回收率为 80.6-105%,相对标准偏差达到 2.6-7.7%。该方法操作简便、分辨率好、环保,能满足婴幼儿补充食品中果蔬泥中顺式-氯氰菊酯对映体残留量的测定要求。

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