牛乳中有机磷农药残留分析方法

将农药残留的气相色谱测定方法开发应用于基质较为复杂的牛乳中，应用丙酮、乙腈（体积比1：4）的混合溶剂提取，离心，收集并浓缩处理样品。此方法的检出限在0．006mg／kg到0．17mg／kg的范围内。牛奶中加标有0．2×10^-6,0．4×10^-6,0．6×10^-6mg／kg三个浓度水平，回收率为87．86％～113．77％；标准偏差〈7％。可以应用此方法监控牛乳样品中有机磷农药残留情况。     

商品奶与原料奶中农药与亚硝酸钠残留分析

采用高效气相色谱(GC)分析法对商品奶和原料奶中农药和亚硝酸钠残留进行分析,并分析不同饲养模式对原料奶中农药残留的影响。结果表明:在所测定的5种农药中,甲胺磷、敌敌畏和马拉硫磷等3种农药残留检出率较高,商品奶为45.0%～67.5%,原料奶为46.8%～71.2%。商品奶和原料奶中甲胺磷、敌敌畏、敌百虫、马拉硫磷和倍硫磷检出率和残留量差异不显著(P﹥0.05);而商品奶和原料奶中亚硝酸钠检出率和残留量差异极显著(P﹤0.01)。原料奶中5种农药加权平均检出率、农药加权平均残留量和加权残留总量均为规模化饲养显著低于农户散养和合作社饲养(P﹤0.05),后两者之间无显著差异(P﹥0.05)。     

Chlorinated pesticide residues in milk of Iranian nursing mothers.

One-hundred-thirty-one samples of human milk were collected during October, 1974, to January, 1976, throughout the Tehran area. Sources included four maternity hospitals as well as individual nursing mothers outside of hospitals. The samples were collected 1 to 8 days after child birth from women 14 to 42 yr old and from all social strata. The samples were analyzed for chlorinated pesticide residues by gas-liquid chromatography. Insecticides 1,1,1-trichloro-2,2-bis(p-chlorophenyl)ethane (DDT) (with its metabolites), isomer of benzene hexachloride (gamma BHC), and dieldrin were detected in varying concentration in 101, 108, and 47 samples, respectively. The means and ranges were .024 (.001 to .333) ppm, .008 (.001 to .046) ppm, and (.001 to .028) ppm. These concentrations in human milk represented insecticidal ingestion by infants. The mean dieldrin exceeded the World Health Organization limit and may pose a health hazard. There was no significant relationship between economic status of donors and pesticide in the milk; however, milk from the older nursing mothers contained more DDT than that from young mothers.     

Persistent organochlorine pesticide residues in milk and dairy products in India

Monitoring of milk and dairy product samples of various brands from different cities in Maharashtra, India, was carried out to determine if there is any contamination due to organochlorine pesticide residues. The measurements were made using a gas chromatograph-electron capture detector system. Trace levels of DDT and HCH were detected in the samples. Total HCH levels in milk and milk product samples were lower than total DDT levels, which could be attributed to earlier extensive antimalaria sanitary activities. Butter had higher levels of DDT than cheese and milk powder. All levels of organochlorine pesticide residues in milk and milk products were well below the maximum permissible limits given by the FAO/WHO. More importantly, as compared with an earlier report, present levels of the contaminants are substantially lower, which indicate the gradual phase out of these compounds.     

Organochlorine pesticide residues in cow's milk from a tropical region of Mexico

A monitoring study was conducted to assess the magnitude of DDT [(1,1,1-trichloro-2,2-bis( p -chlorophenyl)ethane)] and HCH (hexachlorocyclohexane) contamination of bovine milk from the central tropical region of Mexico as the chemicals are extensively used in livestock and public-health programmes. Among pesticide residues analysed, the milk samples collected from Tlalixcoyan showed a mean level of γ-HCH (0.128 mg kg -1 ), which was significantly higher than residues in milk samples from Medellin (0.049 mg kg -1 ) and Paso San Juan (0.022 mg kg -1 ). The mean level of pp '-DDE in Medellin samples (0.039 mg kg -1 ) was significantly higher than in Paso San Juan (0.018 mg kg -1 ) and Tlalixcoyan (0.024 mg kg -1 ) milk samples. The pp '-DDT mean level from Medellin milk samples (0.089 mg kg -1 ) was significantly higher than the levels detected in the other two areas. The highest mean Σ-DDT level detected in Medellin samples (0.146 mg kg -1 ) was three times the FAO/WHO tolerance level. The highest acceptable daily intakes calculated for Σ-DDT were 0.017 μg kg -1 bw day -1 for adults and 0.530 μg kg -1 bw day -1 for infants; for γ-HCH residues, they were 0.021 μg kg -1 bw day -1 for adults and 0.666 μg kg -1 bw day -1 for infants, indicating that infants are more exposed to pesticide residues. Results indicate that cattle exposure to HCH and DDT results in high levels in dairy milk and a potential health risk for consumers.     

Analysis of contaminated milk with organochlorine pesticide residues using gas chromatography

Milk and milk products are considered to have tremendous nutritional values as they contain a good proportion of protein, fats, and important minerals. However, the nutritional value of the milk produced in Pakistan is not up to the mark as extensive use of pesticides on crops resulted in contamination of milk. Consumption of contaminated food such as milk, meat, fish, eggs can induce increased proportion of organochlorine pesticides in the body. The purpose of this study is to determine organochlorine pesticide residues in milk and their toxicity level by Maximum Residues Level (MRL) values. In the current study, organochlorines such as Dichlorodiphenyltrichloroethane (DDT), Dichlorodiphenyldichloroethane (DDE), Dieldrin, Gamma-hexachlorocyclohexane (?-HCH) also known as Lindane, α-Endosulphan, β-Endosulphan and Endosulphan sulphate were detected with the help of gas chromatograph equipped with electron detector. These pesticides were confirmed by using gas chromatography-mass spectrometry (GC-MS). Analysis of variance is applied (ANOVA) to determine variations of pesticides in all milk samples. Analysis showed non-significant results (p > 0.05) with large variation among all milk samples regarding pesticide residues. The mean values of DDT, DDE were found to be below the MRL value. The mean values of Dieldrin, ?-HCH were also below MRL value. On the other hand mean values of α-Endosulphan, β-Endosulphan, and Endosulphan sulphate were slightly higher than MRL in few milk points. The present study showed large variations of pesticides residues present in milk samples.     

气相色谱法检测牛奶中有机氯类农药残留前处理的优化

目的优化前处理操作,避免样品的前处理问题影响最终定量结果的准确性。方法比较分析了牛奶中农药残留测定的前处理过程中移液器的使用、药品的加入量、样品的提取、样品的浓缩程度、旋转蒸发瓶的选择、样品的洗涤提取、样品的净化等操作步骤,对色谱图中杂质及加标回收率的影响。结果规范优化前处理过程后,平均回收率由75.43%提高至92.64%,平行样的相对标准偏差由8.48%降低至2.02%,减少了杂质对样品的影响。结论该方法前处理优化后,检测方法更为准确、有效,适合测定牛奶中的有机氯类农药残留。     

Determination of pesticide residues in milk using a QuEChERS-based method developed by response surface methodology

Response surface methodology (RSM) was employed to optimise a rapid and easy sample preparation method for the determination of 14 different pesticide residues in milk. The recovery of each pesticide was investigated by a QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe)-based method with respect to 3 variables, the amounts of sodium acetate (Na Acetate), primary secondary amine (PSA), and octadecylsilane (C₁₈). After optimisation, the maximum predicted recovery was the 99.73% rate for myclobutanil under the optimised conditions of 1.70 g Na Acetate, 600.00 mg PSA, and 489.96 mg C₁₈. The recovery rates of the other 9 hydrophilic pesticides were ranged from 82.01% to 98.84%. However, the recovery rates for the 4 lipophilic pesticides (2,4′-DDE, 4,4′-DDE, 2,4′-DDT, and 4,4′-DDT) were <80% because they were removed by C₁₈ along with the other fatty compounds. This method could be implemented in many laboratories to reduce inspection time and cost.     

Organochlorine pesticide residues in bamboo shoot

BACKGROUND: Xenobiotic organochlorine pesticides (OCPs) are a major environmental problem because of their historic widespread use, pronounced persistence against chemical and biological degradation, and bioaccumulation in the food chain. Pesticide use is prevalent in the production of edible bamboo shoots, which are exported widely from China. To evaluate the quality of Chinese bamboo shoots we determined the residual content of some OCPs in shoot samples. RESULTS: Three types of OCPs—hexachlorocyclohexane (HCH), 1,1,1‐trichlor‐2,2‐bis(p‐chlorophenyl)ethane (DDT) and pentachloronitrobenzene (PCNB)—were detected in bamboo shoots from Zhejiang province, China. Detection rates were 100%, 100% and 75% for HCH, DDT and PCNB, respectively. However, the average residue concentration did not exceed the maximum residue limit for pesticides detected in food in China (50 µg kg^?1). In terms of residue concentrations of the pesticides, 82.14% of the bamboo shoot samples could be classified as safe. CONCLUSION: While all sampled bamboo shoots contained OCP, most (82.14%) were safe for consumption. Copyright © 2010 Society of Chemical Industry     

食醋中有机磷农药残留的测定

用气相色谱法(GC)分析测定并采用凝胶色谱净化(GPC)系统预处理,建立了食醋中有机磷残留量的检测方法。样品用乙腈提取,经凝胶渗透色谱柱净化,再经中等极性的毛细管色谱柱DB-1701P(30m×0.25mm×0.25μm)分离,气相色谱火焰光度检测器(FPD)检测。有机磷在食醋样品中的残留量检测的检出限为0.0040～0.050mg/kg。在样品中添加29种农药混合标准溶液,平均回收率为72.4%～120.8%,相对标准偏差为0.7%～14.5%(n=3),可满足食醋样品中有机磷农残的测定。     

芹菜农药残留风险评估

目的 评估芹菜样品的农药残留风险,为生产上安全合理使用农药及制订农药最大残留限量标准提供参考依据.方法 随机抽取基地30份芹菜样品,检测68种农药残留,分别运用风险系数法、慢性膳食摄入风险(acceptable daily intake,ADI)评估法、急性膳食摄入风险(acute reference dose,ARf...     

葡萄酒酿造过程中农药残留的变化

本文综述了国内外葡萄酒酿造过程对农药残留的影响,重点讨论了原料除梗破碎、浸渍、发酵、倒灌、下胶澄清和过滤等过程对农药残留的迁移规律及代谢产物的影响,并对今后该领域的发展前景进行了展望,为葡萄酒生产中减少农药残留、保障消费者食品安全提供一定的参考。     

气相色谱法在农药残留分析中的应用

固相萃取是目前常用的一种样品预处理方法, 它具有高效、快速、方便和高选择性等特点.气相色谱是农药和药物残留分析中应用最多的分析检测方法,固相萃取和气相色谱的联用实现了样品前处理及分离分析的优化组合.综述了固相萃取和气相色谱联用技术在农药残留分析中的应用.     

茶叶中农药残留的检测

为了更好地解决茶叶中的农药残留问题,利用气相色谱仪(具电子捕获检测器)对茶叶中的α-HCH、β-HCH、γ-HCH、δ-HCH、ρ,ρ'-DDE、o,ρ'-DDT、ρ,ρ'-DDD和ρ,ρ'-DDT等农药的残留进行了测定,同时介绍了样品的处理方法,给出了测试的要求及部分样品测试的色谱图。结果表明:部分茶叶中有农药残留,总含量在100μg/L左右。     

Organochlorine pesticide residues in archived UK soil

Archived background soils ("Broadbalk', 1944-1986) and sludge-amended soils ("Luddington", 1968-1990), collected from long-term agricultural experiments in the UK, were analyzed for a range of organochlorine (OC) pesticides to establish trends over time. Concentrations typically ranged from 0.1 to 10 ng/g of soil (dry weight), with gamma-hexachlorocyclohexane (gamma-HCH), dieldrin, and p,p'-DDE consistently having the highest concentrations. The trends in the Broadbalk background soils are largely consistent with usage patterns, with peak concentrations occurring in the 1960s for DDTs and between the 1960s and the 1980s for the other OCs. In the Luddington control and sludge-amended soils, several of the OCs show a significant decline in concentrations from the late 1960s to 1990, with half-lives ranging from approximately 7 years (alpha-HCH) to approximately 25 years (dieldrin). The sludge-amended plot received 125 tonnes of sludge per ha in 1968, which was mixed in to a depth of 15 cm. It appears that the sludge treatment had little effect on concentrations in the soil, with no significant difference between control soil and sludge-amended soil for most compounds, except for HCB, p,p'-DDE, and dieldrin. Enantiomeric fractions (EFs) of some chiral pesticides (alpha-HCH, cis- and trans-chlordane, and o,p'-DDT) were determined in the Luddington soils. Results reveal that enantioselective degradation of OC pesticides is occurring in these soils for trans-chlordane (TC) and cis-chlordane (CC). However, the depletion over time is not statistically significant, and there is no statistically significant difference between EFs in the control soil and sludge-amended soil. This indicates that enantioselective microbial degradation was not consistent over time and that the addition of sludge to soil did not significantly alter the enantiomeric preference of the microbial community.     

销售蔬菜中农药残留分析

为了解沈阳市蔬菜农药残留情况,随机采集43种蔬菜,共1180份样品,采用快速检测法和气相色谱法进行检测.43种蔬菜中,检测出农药残留超标的蔬菜有:茄子、芹菜、小白菜、菠菜和油麦菜,主要的残留农药是氧化乐果、磷胺、水胺硫磷、对硫磷、甲拌磷、三唑磷;蔬菜的农药残留受季节影响明显,冬季蔬菜农药残留最为严重;根据蔬菜种类比较发现,叶菜类蔬菜的农药残留问题明显大于果菜类和根茎类蔬菜.     

Organochlorine pesticide residues in meat of various species

The quantity of organochlorine pesticides present in pork, rabbit, chicken, turkey and horse meat was determined. Levels of residual pesticide were rather higher in the latter three species than in the former two. They were not closely related to fat content.     

食品中农药残留筛查系统的构建

对常见农药的种类、农药残留的危害及有关农药残留的最新检测技术和复杂基质样品的前处理技术进行概述,主要总结固相萃取、凝胶渗透色谱、微波辅助消解以及分散固相萃取技术。农药残留检测主要使用色谱学方法,文中重点概述气相色谱、液相色谱方法以及相应的质谱联用技术,高分辨质谱技术的发展可以为农药残留筛查系统的建立提供有力支撑。在此基础上提出基于粮油食品中重点关注的农药残留种类并建立农药残留的监测系统、软件系统及数据库,进而建立农药残留的风险筛查系统,为政府部门及产业部门掌握农产品农药污染情况提出切实可行的解决方案。