液液萃取-气相色谱-质谱联用快速检测葡萄酒中14种农药残留

建立了葡萄酒中14种农药残留的气相色谱-质谱联用选择离子模式进行监测的检测方法,样品采用正己烷∶乙酸乙酯（1∶1）萃取,无需净化。该方法在0.01～10 mg/L范围内线性关系良好,相关系数大于0.998;在0.01～1.0 mg/L添加水平范围内,平均加标回收率在90.32～108.13之间;最低检出限（LOD）在0.01～0.10 mg/kg之间,定量检出限（LOQ）为0.001～0.05 mg/kg,相对标准偏差均小于10%。     

冷冻干燥和热风烘干对菠菜中农药残留的影响

食品安全的控制贯穿从农场到餐桌的全过程,涉及源头生产、流通、加工和销售等阶段。冷冻干燥和热风干燥是常用的干制菠菜方法,文中研究了真空冷冻干燥和热风干燥对菠菜中有机磷和拟除虫菊酯类农药的影响。实验结果表明:不同农药种类在冷冻干燥和热风干燥中的损失不同,有机磷农药比拟除虫菊酯类农药的损失大,与有机磷农药的蒸汽压较高、稳定性差相关。冻干过程对农药造成的损失与农药的溶解度有关,而烘干过程对农药造成的损失与农药的蒸汽压和热稳定性有关。试验农药中溶解度最大的乐果在冻干过程中损失最小,而蒸汽压最大的马拉硫磷在烘干过程中损失最大。     

高效液相色谱-DAD法检测粮谷作物中多种菊酯类农药残留

建立了同时分离检测粮谷作物中菊酯类杀虫剂(胺菊酯、三氟氯氰菊酯、高效氯氰菊酯、四氟甲醚菊酯和氰戊菊酯)的高效液相色谱(HPLC)–二极管阵列检测器(DAD)法。结果表明,5种农药在15.5 min内实现了基线分离,检出限在0.01~0.05μg/m L之间。该方法是高效、灵敏、快速检测粮谷及其它样品中菊酯类农药残留的有效方法。     

Non-targeted screening of pesticides for food analysis using liquid chromatography high-resolution mass spectrometry-a review

ABSTRACT

Targeted liquid chromatography-tandem mass spectrometry (LC-MS/MS) is a robust and reliable tool in quantitative analysis of pesticide residues in food samples. However, these methods have been only targeted to a predefined set of pesticides. Many other unexpected pesticides and/or their (bio)transformation products present in food matrices that may be harmful to consumers need to be discovered for food safety monitoring purpose. Therefore, non-targeted screening approaches using liquid chromatography coupled to high-resolution mass spectrometry (LC-HRMS) have gained much attention in food monitoring recently. However, the development and implementation of non-targeted screening of potential pesticides and their (bio)transformation products in food samples are particularly challenging due to the inherent sample complexity and large quantity of MS data. To provide guidance on how to use non-targeted screening approaches for pesticide screening, three different aspects, namely, sample preparation, data acquisition and data processing, encompassed in the workflow of non-targeted screening approaches have been discussed, and current strategies, advances and challenges regarding these three aspects are reviewed. In addition, the recent application of non-targeted screening analysis of pesticide residues and their (bio)transformation products in food samples has been overviewed in this paper.     

蔬菜水果中有机磷农药的基质效应分析及检测方法选择

目的 通过对常见蔬菜水果中有机磷农药的基质效应进行全面的分析, 探索更加高效的有机磷农药残留检测手段。方法 30种(11类)供试蔬果样品分别利用乙腈提取, 经QuEChERS净化后, 配制溶剂标准工作曲线和基质标准工作曲线, 利用气相色谱-串联质谱(GC-MS/MS)和超高效液相色谱-串联质谱(UPLC-MS/MS)分析19种有机磷农药的基质效应表现。结果 利用GC-MS/MS分析得到的19种有机磷农药的溶剂标准曲线及其30套基质标准曲线在10~200 μg/L浓度范围内线性关系良好, 利用UPLC-MS/MS分析得到的19种有机磷农药的溶剂标准曲线及其30套基质标准曲线在4~100 μg/L浓度范围内线性关系良好, 所有工作曲线的线性相关系数(r2)均大于0.99; 利用GC-MS/MS分析时, 大部分供试农药在供试基质中呈较强的基质增强效应, 其中水胺硫磷的基质效应最强, 西葫芦可以有效校正供试农药的基质效应; 利用UPLC-MS/MS分析时, 供试农药以弱基质效应表现为主, 西葫芦对供试农药基质效应的校正能力不明显。结论 在利用GC-MS/MS检测供试有机磷农药时, 可用西葫芦配制基质匹配标准溶液进行定量分析; 在利用UPLC-MS/MS检测供试有机磷农药时, 除了乙酰甲胺磷、乐果、敌敌畏、亚胺硫磷, 其他农药均可利用溶剂标准溶液进行定量分析。     

食品中敌菌灵残留量的HPLC测定方法研究

建立了一套较为完善的检测食品中农药敌菌灵残留量的高效液相色谱外标法。采用乙腈-水溶液为流动相,流速1.0ml/min。于250nm用紫外检测器进行检测。其重复测定结果的RSD在2.60%～4.80%范围内,回收率在90.50%～103.66%范围内。本方法适用于蔬菜和原粮中敌菌灵农药残留量的测定。     

Allethrin Promotes Apoptosis and Autophagy Associated with the Oxidative Stress-Related PI3K/AKT/mTOR Signaling Pathway in Developing Rat Ovaries

The increased concern regarding the reduction in female fertility and the impressive numbers of women undergoing fertility treatment support the existence of environmental factors beyond inappropriate programming of developing ovaries. Among these factors are pyrethroids, which are currently some of the most commonly used pesticides worldwide. The present study was performed to investigate the developmental effects of the pyrethroid-based insecticide allethrin on ovarian function in rat offspring in adulthood. We mainly focused on the roles of oxidative stress, apoptosis, autophagy and the related pathways in ovarian injury. Thirty-day-old Wistar albino female rats were intragastrically administered 0 (control), 34.2 or 68.5 mg/kg body weight allethrin after breeding from Day 6 of pregnancy until delivery. We found that allethrin-induced ovarian histopathological damage was accompanied by elevations in oxidative stress and apoptosis. Interestingly, the number of autophagosomes in allethrin-treated ovaries was higher, and this increase was correlated with the upregulated expression of genes and proteins related to the autophagic marker LC-3. Furthermore, allethrin downregulated the expression of PI3K, AKT and mTOR in allethrin-treated ovaries compared with control ovaries. Taken together, the findings of this study suggest that exposure to the pyrethroid-based insecticide allethrin adversely affects both the follicle structure and function in rat offspring during adulthood. Specifically, allethrin can induce excessive oxidative stress and defective autophagy-related apoptosis, probably through inactivation of the PI3K/AKT/mTOR signaling pathway, and these effects may contribute to ovarian dysfunction and impaired fertility in female offspring.     

Retinal Toxicity Induced by Chemical Agents

Vision is an important sense for humans, and visual impairment/blindness has a huge impact in daily life. The retina is a nervous tissue that is essential for visual processing since it possesses light sensors (photoreceptors) and performs a pre-processing of visual information. Thus, retinal cell dysfunction or degeneration affects visual ability and several general aspects of the day-to-day of a person’s lives. The retina has a blood–retinal barrier, which protects the tissue from a wide range of molecules or microorganisms. However, several agents, coming from systemic pathways, reach the retina and influence its function and survival. Pesticides are still used worldwide for agriculture, contaminating food with substances that could reach the retina. Natural products have also been used for therapeutic purposes and are another group of substances that can get to the retina. Finally, a wide number of medicines administered for different diseases can also affect the retina. The present review aimed to gather recent information about the hazard of these products to the retina, which could be used to encourage the search for more healthy, suitable, or less risky agents.     

气相色谱-三重四极杆质谱法测定稻米中27种持久性有机污染物

目的 建立气相色谱-三重四极杆质谱法测定稻米样品中多氯联苯、有机氯农药和多溴联苯醚等27种持久性有机污染物的分析方法。方法 糙米粉样品经水化后,采用乙酸乙酯进行2次直接提取,采用5 g酸性硅胶(44%,m:m)固相净化柱进行净化后采用气相色谱-三重四极杆质谱在动态多反应离子监测模式进行分析,内标法定量。结果 27种持久性有机污染物中,4-溴联苯醚的回收率较低,其他7种多氯联苯、7种有机氯农药和12种多溴联苯醚具有较好定量范围,其中高取代溴联苯醚呈二次曲线,回归系数均大于0.996;方法检出限为0.002～1.543 ng/g之间,高取代溴联苯醚的检测灵敏度略差;方法回收率为59.3%～132.7%,相对标准偏差为0.7%～10.8%(n=6)。结论 本方法样品前处理操作简单,具有较好的灵敏度、准确度和精密度,适用于稻米中极低含量持久性有机污染物的检测分析。     

基于USB的有机磷农药检测系统设计

为实现在农业生产中对有机磷农药的残留量进行快速有效地检测,设计了一种基于USB的有机磷农药检测系统。首先简单介绍了有机磷农药检测系统的工作原理,然后利用ARM微控制器实现数据采集,并通过USB与上位机PC机通信,实现下位机与上位机数据的实时传输,最终实现有机磷农药检测系统的功能,该系统可以有准确有效地检测出溶液中有机磷农药的残留量。