用手持式农药速测仪酶法现场测定蔬菜中有机磷及氨基甲酸酯农药残毒

检测蔬菜中有机磷类及氨基甲酸酯类农药残留通常采用气相色谱、色谱-质谱联用[1]等方法, 不适应现场快速检测的要求. 关于快速分析方法, 国外主要采用电化学酶传感器法[2], 还有微孔板酶标仪法[3]. 前者存在电极易受污染且需再生处理的麻烦; 后者难以实现现场检测. 国内报道的有酶抑制光度法[4]、单点目视比色法及速测卡法等, 其中目视比色法和速测卡法虽然具有操作简便等优点, 但由于实验误差较大, 灵敏度较低, 只能作为定性分析. 本文在前期工作的基础上[5,6], 研制了一种体积小(140 mm×70 mm×30 mm)、重量轻(整机180 g)、能耗低(电池可连续使用50 h)且现场实用的手持式农药残毒速测仪, 开发了专用试剂包并建立了蔬菜中有机磷类及氨基甲酸酯类农药残毒的现场分析方法, 对6种蔬菜及速冻玉米样品进行了实际检测, 并与GC-MS方法[1]进行了对照, 结果令人满意.     

白术中有机磷及氨基甲酸酯类农药残留量的测定

对白术中21种有机磷和氨基甲酸酯类农药残留量进行同时测定。在超声波辅助下溶剂提取,弗罗里硅土和中性氧化铝层析柱净化,选择离子-气相色谱-质谱(SIM-GC-MS)联用检测。农药混标在0.005~1.0μg/mL的浓度范围内线性良好,在0.2、0.05μg/mL两个水平添加回收率分别为81.2%~108.6%和89.8%~124.2%,相对标准偏差分别为4.6%~8.7%和5.3%~10.7%。本方法快速、灵敏、准确、可靠,可作为中草药中多种农药残留同时检测的一种方法。     

GC-NPD同时测定中草药中有机磷和氨基甲酸酯农药残留量

建立了中草药中有机磷和氨基甲酸酯类农药残留量同时检测的气相色谱分析方法.中药材试样依据正交实验的优化条件,用V(C6H14):V(丙酮)=1:1混合提取剂进行超声波提取,经弗罗里硅土和中性氧化铝层析柱净化后,采用HP-5毛细管柱分离,氮磷检测器同时检测中草药中15种有机磷和7种氨基甲酸酯类农药残留量.22种农药在0.015～1.0 mg/L范围内线性良好,线性相关系数为0.9950～1.000,在0.05、0.1 mg/kg两个添加水平的平均回收率分别为70.6%～128.6%和69.5%～116.1%,相对标准偏差分别为0.98%～18%和0.37%～15%.各种农药的检出限为0.002～0.015 mg/L.方法已用于中草药中有机磷和氨基甲酸酯类农药残留量的同时检测.     

中草药中有机磷及氨基甲酸酯类农药残留量的GC-MS测定

气相色谱-质谱法同时测定中草药中多种有机磷及氨基甲酸酯类农药残留量.采用V(乙腈)∶V(丙酮)＝3∶7混合溶剂微波辅助提取,弗罗里硅土和中性氧化铝层析柱净化,气相色谱-质谱(GC-MS)联用检测,农药混标在0.01～1.0 μg/mL范围内线性良好,在0.5、0.1、0.05 μg/mL 3个水平添加平均回收率分别为86.5%～110.6%、81.2%～108.3%和72.9%～122.3%,相对标准偏差分别为2.6%～8.3%、4.6%～9.7%和2.3%～10.7%.     

蔬菜中有机磷和氨基甲酸酯类农药多残留联合检测方法

有机磷和氨基甲酸酯类农药是蔬菜生产中常用的杀虫剂,我国70%的有机磷杀虫剂是剧毒、高毒农药。农药如果使用不当,不但药效不好,还会发生药害,污染环境,造成人畜中毒。因此,加强对农药残留的监控,禁止农药残留超标的蔬菜进入市场,确保消费安全已成为当务之急。本文报道用毛细管气相色谱法测定蔬菜中有机磷和氨基甲酸酯类农药多残留的联合检测方法。     

植物酯酶应用于有机磷农药残留分析技术的研究进展

有机磷农药残留在食品中,进入人体危害人类健康.因此,快速而灵敏的检测技术是预防农药残留危害的前提条件.而酶抑制技术正是一项快速检验技术.本文作者介绍了农药残留分析的现状,详细分析了植物酯酶应用于农药残留分析技术的研究进展.     

用于测量农药残留的小麦酯酶的选择

为研制探测农药残留的生物传感器，研究了农药乐果[O,O-二甲基S－（N－甲基胺基甲酰甲戎）二硫代磷酸酯]对各种小麦植物酯酶的抑制，从小麦中提取植物酶，以农药乐果为抑制剂，采用分光光度法研究了乐果对各种小麦酯酶活性的影响；研究显示，不同品种小麦酯酶对农药乐果的敏感度不同，在所研究的品种中，豫麦39和小麦周9对乐果较敏感，研究结果说明了选择小麦酶源的必要性。     

双毛细管气相色谱法测定果蔬中有机磷及氨基甲酸酯类农药残留

对果蔬样品中残留的有机磷及氨基甲酸酯农药,通过较为简便有效的提取方法,以双毛细管柱气相色谱法进行测定,排除了干扰影响,增加了试验结果的可靠性,取得了满意结果。     

色谱法分析氨基甲酸酯类农药残留的研究进展

概述了近年来检测氨基甲酸酯类农药残留的前处理技术与色谱方法的研究进展.     

基于乙酰胆碱酯酶抑制的有机磷农药生物传感器研究进展

有机磷农药(OPs)残留可通过食物链在生物体内富集,从而对自然生态和人类健康带来极大威胁.用于检测有机磷农药的传统分析方法(如高效液相色谱法和气相色谱法)具有响应时间较长、成本较高以及检测程序复杂等局限.近年来,生物传感因具有专一性强、速度快、准确度高等优势被广泛用于分析领域.而利用乙酰胆碱酯酶(AChE)作为识别元件...     

Simultaneous Determination of Carbamate and Organophosphorus Pesticides in Honeybees by Liquid Chromatography-Mass Spectrometry

Summary The potential of liquid chromatography-mass spectrometry (LC-MS) has been studied for the simultaneous determination of sixteen carbamate and organophosphorus pesticides in honeybees using a traditional sample preparation protocol based on acetone extraction and dichloromethane partitioning. The performances of both atmospheric pressure chemical ionization (APCI) and electrospray (ES) interfaces were compared. APCI offered better sensitivity and specificity for a higher range of pesticides. Limits of quantification were from 0.01 to 0.17 mg kg^–1, at which recoveries obtained were between 64 and 93%, except for pirimicarb that was at 13%, with relative standard deviations ranging from 7 to 20%. Fenitrothion, fenoxycarb, methiocarb and phoxim were found in bees from Valencian Community beehives at concentrations between 0.03 and 3.75 mg kg^–1.     

液相色谱串联质谱法测定烟草中有机磷和氨基甲酸酯类农药残留量

用乙腈对烟末样品进行提取,提取液经乙二胺-N-丙基硅烷吸附剂净化后,采用高效液相色谱-串联质谱法检测,在20min内完成了40种有机磷和氨基甲酸酯类农药的定量分析。40种农药的平均回收率为72%～113%,相对标准偏差为1.2%～13%,检出限为0.49～19.7μg/kg。该方法的回收率、重复性及检出限均能满足烟草农药残留分析的要求。     

气相色谱法测定小麦粉中有机磷类和拟除虫菊酯类农药残留量

应用气相色谱法测定了小麦粉中4种有机磷和拟除虫菊类农药的残留量.样品中的残留农药用乙腈提取分离,所得提出液减压蒸发至近干,再用吹氮法蒸干.残渣用正己烷-乙酸乙酯(9+1)混合溶液2 mL溶解,所得溶液经中性氧化铝固相萃取柱净化.收集洗脱液,再用上述混合溶液10 mL淋洗固相萃取柱,收集洗脱液与上次洗脱液合并,减压蒸发至...     

Automatic Electronic Tongue for On-Line Detection and Quantification of Organophosphorus and Carbamate Pesticides Using Enzymatic Screen Printed Biosensors

This work presents an automatic system, based on an electronic tongue, for resolution of mixtures of three pesticides. Inhibition detections were performed during the steady state of biosensors response. Three biosensors were built using two enzymes, electric eel (EE), genetically-modified Drosophila melanogaster (B131), and electric eel co-immobilized with drosophila melanogaster (BH). Calibrations curves for paraoxon, dichorlvos, and carbofuran were performed in the ranges 0.4–50.4 µM, 0.01–1.01 µM, 0.01–0.41 µM with LOD of 3.91 × 10^?8, 6.30 × 10^?11, and 5.84 × 10^?10, respectively. An artificial neural network (ANN) was used to model the combined response of three pesticides. A set of 19 mixtures were prepared in order to train the artificial neural network, the modeling was validated with a set of 6 spiked samples of river water. The error and recovery yields were found in consistent with expected values.     

分散固相萃取-液相色谱-质谱检测蔬菜水果中氨基甲酸酯和有机磷农药

以乙二胺-N-丙基硅烷(PSA)为吸附剂,乙腈为萃取溶剂,建立新型的基质分散固相萃取农残样品前处理技术,实现样品快速制备;利用LC-MS同时定量蔬菜和水果中的氨基甲酸酯和有机磷农药,并与常用固相萃取吸附剂ODS进行对比。选取4种代表性的蔬菜和水果,采用加标回收的方法,测定回收率和精密度,检验该方法的准确性和可靠性。对于绝大多数农药,在不同基质中,回收率为80%~110%,精密度为0.3%~8.0%。以西红柿为基质,检出限可达0.5~35μg/kg。研究表明,本方法法简单、快速、经济并具有较高灵敏度。采用本方法可对当地市场上常见时令蔬菜及水果进行监测。     

对几种氨基甲酸酯类农药的荧光特性研究

研究了有机物分子结构与荧光产生之间的关系。利用这一理论分析了西维因、克百威、残杀威等几种常用的氨基甲酸酯类农药的分子结构并揭示了它们的荧光光学特性,从而确定了氨基甲酸酯类农药产生荧光的特性,为进一步利用荧光分析法对氨基甲酸酯类农药进行检测提供理论依据。并且利用稳态荧光光谱仪对西维因和克百威标准溶液进行了荧光光谱实验,结果表明,氨基甲酸酯类农药在一定的溶剂条件下是能够受激发荧光的,是可以利用荧光光谱分析法来对它们进行检测．     

Developments in the Determination of Organophosphorus Pesticides

Abstract

In this paper, a review is given of some recent developments in organophosphorus pesticides residue methodology. Enrichment on XAD-resins or C₁₈ bonded phases, clean-up by gel permeation and determination by high-performance liquid chromatography (HPLC) with specific detectors can be considered as the major fields of development in the past years.

Despite of the progress made, there is still a further need for procedures which reduce handling time, e.g. by automation, and/or increase specificity of the HPLC determination in matrices of practical interest, such as food, animal and human tissues and environmental samples.     

有机磷农药酶生物传感器研究进展

酶生物传感器（EBS）以简单、廉价、易于微型化等优势成了有机磷农药（OPs）传统分析方法的最佳替代品。本文从识别OPs的酶及识别机理、电化学EBS、酶的固定化技术、高分子材料的酶固定载体不同角度综述了有机磷农药酶生物传感器研究近况,并重点介绍了一次性丝网印刷酶电极。     

Laser Mass Spectrometry of Organophosphorus Pesticides and Related Compounds

Abstract

Laser mass spectra obtained for 20 organophosphorus (OP) compounds were systematically evaluated for groups containing analogous structural features. Variations in fragmentation can be understood based on simple organic reactions. While detailed mechanistic interpretations of the laser mass spectra (LMS) were not possible, the qualitative features in the LMS obtained from five compounds, not in the original set, could be predicted based on the characteristics of the other OP compounds studied. The success of the prediction lends credence to the qualitative models developed for rationalizing the LMS. A specific feature in the LMS of aromatic thionophosphates is a thiono-thiolo rearrangement. Detailed investigation into the phenomena involved comparison of LMS obtained from aromatic thionophosphates with spectra from electron impact, chemical ionization, field desorption, and secondary ion mass spectrometry. These results led to the conclusion that the rearrangement in laser mass spectrometry must occur during volatilization while the molecule/ion is in the “cloud” present immediately above the laser impact area.