40%毒死蜱微乳剂的高效液相色谱法分析

采用ODS–C18反相色谱柱,用高效液相色谱法测定40%毒死蜱微乳剂制剂含量。方法的相关系数为0.9998,标准偏差为0.0242,变异系数为0.06%,平均回收率为98.6%。     

30%毒·灭乳油(顽虫净)高效液相色谱分析

采用反相高效液相色谱法 ,以甲醇 +水 =70 +30 (v/v)为流动相 ,用紫外检测器对毒死蜱·灭多威乳油进行分离和测定。结果表明 :毒死蜱和灭多威含量测定的精密度标准偏差分别为0 0 7和 0 0 5 ;变异系数分别为 0 35 %和 0 5 0 % ,回收率分别为 98 99%～ 10 1 0 2 %和 99 6 4%～10 1 95 % ,线性相关系数分别为 0 9999和 0 9996。     

毒死蜱中间体三氯吡啶酚的合成

选择吡啶路线合成了毒死蜱的中间体三氯吡啶酚。以吡啶为原料,经氯化、还原及水解3步反应得到目标化合物,含量、收率均达到92.5%。     

林地腐殖土腐植酸对毒死蜱水解影响及吸附作用

采用平衡振荡法研究腐植酸对毒死蜱水解的影响和毒死蜱在腐植酸上的吸附特征及其影响因素.结果表明,在试验浓度范围内腐植酸可促进毒死蜱的水解,腐植酸浓度为120 mg/L时,毒死蜱的水解速率常数k明显增大,为不加腐植酸时的2.53倍,腐植酸浓度增加毒死蜱的水解速率降低.毒死蜱在腐植酸上的吸附行为均可用Linear方程和Freundlich方程来描述,拟合效果均达到显著水平;试验条件下温度为15℃时毒死蜱在腐植酸上的吸附量最大,随温度的升高吸附量呈现出先降低后增大的趋势;pH值减小,腐植酸对毒死蜱的吸附能力增大;而离子强度对毒死蜱的吸附影响不明显;腐植酸添加量越大,吸附量越大,但单位质量的腐植酸吸附量越小.     

三唑磷·毒死蜱乳油的液相色谱分析

以ODS色谱柱,UV246 nm为检测波长,用甲醇:水=90∶10(V/V)作为流动相,在ODS色谱柱上同柱液相色谱法测定三唑磷、毒死蜱的含量。方法的变异系数三唑磷为0.41%,毒死蜱为0.35%,三唑磷的回收率为98.9~100.7%,毒死蜱回收率为99.5%~100.6%。相关系数三唑磷为0.9968,毒死蜱为0.9999。     

Polymeric sodium alginate interpenetrating network beads for the controlled release of chlorpyrifos

Novel polymeric sodium alginate (Na‐Alg) interpenetrating network (IPN) beads have been prepared by crosslinking Na‐Alg blend with gelatin (GE) or egg albumin (EA) using glutaraldehyde (GA) as the crosslinking agent. These beads were used for the controlled release of chlorpyrifos. The swelling experiments were performed in water at different temperatures, and these data were used to calculate the molecular mass (M_C) between crosslinks as well as diffusion coefficients. Diffusion coefficients calculated from desorption data were lower by about two orders of magnitude than those calculated from sorption results. Higher values of M_C were obtained for the gelatin‐based IPNs than the neat Na‐Alg and egg albumin‐based matrices. Size of the beads did not vary significantly either by the network or by increasing the exposure time to the crosslinking agent. The scanning electron microscopy (SEM) was used to understand the surface characteristics of the beads. Differential scanning calorimetry (DSC) indicated a molecular level dispersion of chlorpyrifos in the polymer matrix. The percentage entrapment efficiency showed a dependence on the type of network polymer as well as time of exposure to the crosslinking agent. The encapsulation efficiency decreased with an increase in time of exposure to the crosslinking agent. In vitro release experiments have been performed to follow the release kinetics of chlorpyrifos from the matrices. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 85: 911–918, 2002     

A gas chromatography–mass spectrometry method for the detection of chlorpyrifos contamination in palm-based fatty acids

Chlorpyrifos is a Malaysian Pesticide Board-approved organophosphate insecticide, which may become concentrated during fractionation. The objective of this project was to develop and validate a method to detect and quantify chlorpyrifos in food-grade fatty acids ingredients, e.g. caprylic-capric acid mixture and oleic acid (OLA) used to synthesize triacylglyceride based food additives and in the cosmetic industry. A selective ion monitoring gas chromatography–mass spectrometry method with a matrix-matched calibration curve calibration was selected. The method involved the direct injection of chlorpyrifos spiked into the fatty acids matrix. The percentage recoveries at spiking levels of 0.5, 0.75, 2.5, and 4.0 μg g⁻¹ of chlorpyrifos in OLA and caprylic-capric acid ranged from 85.7%–101.1% to 97.2%–112%, respectively, with a relative standard deviation of within 11%. The intra-day and inter-day precision were deemed acceptable as indicated by an relative SD value of within 10%. A good linear relationship with a coefficient of correlation >0.99 for the matrix-matched calibration was achieved between 0.5 and 5 μg g⁻¹. The limit of detection and limit of quantification corresponded to 0.5 μg g⁻¹ for OLA and 0.55 μg g⁻¹ for caprylic-capric acid.     

菜心中残留毒死蜱的去除方法研究

针对我国当前蔬菜生产中由于农药的不合理使用而导致的农药残留超标的问题,开展了在对蔬菜农药的残留去除方法的研究。设计了以菜心为材料,以有机磷农药毒死蜱为研究对象,在不同时间、不同温度、不同清洗剂(清水、淘米水、洗洁精、加热、Na2CO3溶液以及Na Cl溶液等)以及不同的浓度下对菜心中毒死蜱残留去除效果的研究探讨。实验结果表明,对菜心中残留毒死蜱的去除效果是:淘米水Na2CO3洗洁精NaCl清水。     

茶叶中联苯菊酯、毒死蜱的测定能力验证结果与分析

目的通过参加能力验证实验,提高实验室农药残留检测的能力。方法优先选择本实验室常用方法,依据NY/T 761-2008、GB/T 23204-2008、GB 23200.13-2016方法,对样品进行相应的提取净化处理,随后根据相应的仪器进行定性定量检测分析,使用仪器比对、方法比对、人员比对、加标回收、质控样品作为质控方法。结果本次能力验证以NY/T761-2008报出检验结果。样品编号为18-U804检测结果为联苯菊酯:0.214 mg/kg, Z比分数为?0.4,毒死蜱为未检出;样品编号为18-Y023检测结果为联苯菊酯为0.582 mg/kg, Z比分数为?0.3,毒死蜱为0.364 mg/kg, Z比分数为?0.6,组织机构判定结果为满意。结论本次能力验证结果为满意,说明本实验室对农药残留的检测能力较好。     

近红外光谱技术用于菠菜中毒死蜱残留的定量分析研究

本实验基于近红外光谱方法对菠菜中农药残留量定量分析情况进行研究,前期实验通过模拟果蔬成分背景,配制了37个有机磷农药毒死蜱浓度为0.005～0.1mg/kg的模拟混合液体样本;后期对经化学处理后的毒死蜱浓度在0.1～3.65mg/kg的36个菠菜萃取液体样品进行定量分析研究.结果表明,近红外光谱法对分析模拟溶液中的毒死蜱及菠菜萃取溶液中的毒死蜱样本均取得良好的预测效果.