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采用新型高效液相色谱法和分光光度法测定有机磷农药

Organophosphorus pesticides determination by novel HPLC and spectrophotometric method.

作者信息

Harshit Dave, Charmy Kothari, Nrupesh Patel

机构信息

Department of Pharmaceutical Analysis, Institute of Pharmacy, Nirma University, Ahmedabad 382 481, Gujarat, India.

Department of Pharmaceutical Analysis, Institute of Pharmacy, Nirma University, Ahmedabad 382 481, Gujarat, India.

出版信息

Food Chem. 2017 Sep 1;230:448-453. doi: 10.1016/j.foodchem.2017.03.083. Epub 2017 Mar 15.

Abstract

The present work describes a novel HPLC and UV-spectrophotometric method for the simultaneous estimation of chlorpyrifos and prophenofos in vegetables and fruits. In UV method, the absorbance of chlorpyrifos and prophenofos was measured at wavelength 277nm and 289nm respectively and quantitation was carried out by first order derivative method. The calibration curve for chlorpyriphos and prophenofos was found to be linear in the range of 6-16μg/mL with correlation coefficient 0.9979 and 0.9993 respectively. The HPLC separation was achieved on Hibar C column (250×4.6mm, 5µ) using mobile phase consist of acetonitrile: water (90:10, v/v) at flow rate 1.0mL/min and the eluent was monitored at 219nm. Pesticides were extracted from the samples by solid phase extraction and liquid-liquid extraction before the analysis. Out of these two extraction methods, solid phase extraction was found more efficient in terms of % recovery as compared to liquid-liquid extraction. The developed method was applied for estimation of chlorpyrifos and prophenofos and it was found that the chlorpyrifos was 0.018mg/kg, which is above maximum residue limits (0.01mg/kg), which might be toxic to body. Prophenofos was not found in any collected samples of vegetables and fruits.

摘要

本研究描述了一种用于同时测定蔬菜和水果中毒死蜱和丙溴磷的新型高效液相色谱法和紫外分光光度法。在紫外法中,分别在波长277nm和289nm处测量毒死蜱和丙溴磷的吸光度,并采用一阶导数法进行定量。毒死蜱和丙溴磷的校准曲线在6 - 16μg/mL范围内呈线性,相关系数分别为0.9979和0.9993。使用由乙腈:水(90:10, v/v)组成的流动相,流速为1.0mL/min,在Hibar C柱(250×4.6mm, 5µ)上实现高效液相色谱分离,并在219nm处监测洗脱液。在分析前,通过固相萃取和液液萃取从样品中提取农药。在这两种萃取方法中,发现固相萃取在回收率方面比液液萃取更有效。所开发的方法用于测定毒死蜱和丙溴磷,结果发现毒死蜱含量为0.018mg/kg,高于最大残留限量(0.01mg/kg),这可能对人体有毒。在采集的任何蔬菜和水果样品中均未发现丙溴磷。

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