英德横石水镇贫困村蔬菜中农药残留及重金属污染分析

本文研究分析了英德横石水镇溪北村蔬菜中的农药残留和重金属污染。选取24个蔬菜样品,采用气相色谱-双火焰光度检测器(GC-FPD)测定蔬菜中的甲胺磷、甲拌磷、特丁硫磷、甲基对硫磷、杀螟硫磷、甲基异柳磷、丙溴磷、伏杀硫磷、敌敌畏、乙酰甲胺磷、治螟磷、氧乐果、乐果、毒死蜱、马拉硫磷、对硫磷、水胺硫磷、杀扑磷、三唑磷和亚胺硫磷等20种有机磷农药残留;采用气相色谱-电子捕获检测器(GC-ECD)测定蔬菜中的α-六六六、β-六六六、γ-六六六、δ-六六六、百菌清、三唑酮、甲氰菊酯、哒螨啉、氯氰菊酯、氰戊菊酯、溴氰菊酯和氟虫腈等12种农药残留;采用原子吸收-石墨炉法测定铅含量;原子荧光分光光度法测定砷和汞含量,结果表明蔬菜样品中均未检出上述32种农药及3种重金属。研究结果可为英德横石水镇溪北村蔬菜质量定位提供理论依据。     

气相色谱-质谱法同时检测饮用水中6种常见农药残留

建立了测定饮用水中的微量敌敌畏、治螟磷、乐果、二嗪磷、甲基对硫磷、杀螟硫磷残留的气相色谱-质谱法检测方法。饮用水样经固相萃取柱富集,以乙酸乙酯洗脱,经气相色谱质谱联用仪定性定量检测。敌敌畏、治螟磷、乐果、二嗪磷、甲基对硫磷和杀螟硫磷的质量浓度在0.01~5.0μg/mL范围内与其色谱峰面积均呈良好线性关系,线性相关系数不低于0.995,敌敌畏、治螟磷、乐果、二嗪磷、甲基对硫磷和杀螟硫磷的检出限分别为0.01,0.01,0.01,0.005,0.005和0.01 mg/kg。敌敌畏、治螟磷、乐果、二嗪磷、甲基对硫磷和杀螟硫磷测定结果的相对标准偏差均小于5%(n=6),重现性均小于10%(n=6),加标回收率在80%~100%之间。试验证明该方法具有操作简单、准确度高、灵敏度高等优点。     

顶空固相微萃取-气质联用快速测定草莓中5种有机磷农药

采用顶空固相微萃取- 气质联用(HS-SPME-GC/MS)技术建立草莓中二嗪农、倍硫磷、杀螟硫磷、乙基对硫磷和乙硫磷5 种有机磷农药的快速测定方法,实验优化了HS-SPME 萃取条件和GC-MS 条件。结果表明：各组分标准曲线方程为：二嗪农y=23.928x+80.891;倍硫磷y=90.368x － 886.061;杀螟硫磷y = 25.992x+123.012;乙基对硫磷y=92.246x － 431.352;乙硫磷y=62.134x+486.49。线性相关系数R 为0.989～0.998,精密度(n = 5)为7.2%～12.7%,方法检出限为5.2～10.7μg/kg,加标回收率为76%～94%。该方法快速、灵敏、准确、试剂用量少,且各项方法学指标符合检测要求,适合作为食品安全监管与检验的标准方法。     

气相色谱法同时测定地表水中倍硫磷、地虫硫磷、对硫磷和马拉硫磷残留量

本文建立液液萃取-气相色谱法测定地表水中倍硫磷、地虫硫磷、对硫磷和马拉硫磷残留量的方法,并对该方法线性、检出限、精密度和加标回收率进行验证。实验表明,本方法前处理操作简便,方法检出限低,加标回收率和精密度满足分析测试要求,适用于地表水中倍硫磷、地虫硫磷、对硫磷和马拉硫磷等有机磷农药的检测。     

进口粮谷中农药残留状况普查与分析

目的根据各进口国粮谷样品农药残留检出情况,确立进口粮谷中重点监测的农药残留品种和评估潜在的农药残留风险。方法采用修改的GB/T 19649-2006和GB/T 20770-2008方法,对粮谷主要进口口岸青岛、深圳和秦皇岛在2010~2014年期间进口的62例大豆、62例大麦和28例大米样品进行了690种农药残留检测,共获得104880个检测数据。结果来自6个进口国的62例大豆样品均未检出农药残留。来自3个进口国的62例大麦样品中,有8例样品检出5种农药,检出率12.9%;其中检出1种农药的样品占4.8%,检出2种农药的样品占6.5%,检出3种农药的样品占1.6%;检出的农药残留水平在10~1000μg/kg范围的占检出总数的85.7%,大于1000μg/kg占检出总数的14.3%。来自6个进口国的28例大米样品中,有5例样品检出5种农药,检出率17.9%;其中检出1种农药的样品占14.3%,检出2种农药的样品占3.6%;检出的农药残留水平低于10μg/kg占检出总数的50.0%,大于10μg/kg占检出总数的50.0%。大麦和大米样品中检出的农药品种为低毒农药的均占80%,检出的农药为中毒农药的均占20%。按照中国最大残留限量(MRL)标准衡量,只有1例大麦样品检出的溴氰菊酯超出标准要求;按照欧盟MRL标准衡量,4例大麦样品检出的杀螟硫磷超出标准要求;按照日本MRL标准衡量,没有样品检出超标农药。结论我国进口粮谷的农药残留检出率低于10%。农药残留水平处于安全水平。但同时也应当加强溴氰菊酯、杀螟硫磷、甲基嘧啶磷、毒死蜱、甲基毒死蜱、丙环唑、嘧菌酯、增效醚的检测,特别是溴氰菊酯和杀螟硫磷农药残留的监控,以保障消费者的食品安全。     

普洱茶中有机磷类农药残留的测定

为建立气相色谱技术同时测定茶叶中多种有机磷农药残留的方法,并用该方法检测来自云南省5 个普洱茶主产区的30 个普洱茶样品中的有机磷农药残留量,为其安全性评价提供科学数据。样品以乙酸乙酯为提取剂经超声波萃取,提取液用活性炭小柱净化,采用气相色谱火焰光度检测器检测,外标法定量。该方法在3 个添加水平下,9 种组分的平均回收率为71.1%～113.8%,相对标准偏差为0.9%～13.3%。方法的检测限为1.0～2.5μg/kg。普洱茶样品检出的农药有敌敌畏、乙酰甲胺磷、乐果、杀螟硫磷、马拉硫磷、喹硫磷、三唑磷,其中杀螟硫磷和乐果的检出率较高,但含量均低于欧盟限量标准。从茶叶中有机磷农药残留量来看,普洱茶具有较高的食用安全性。     

同时测定蔬菜中15种有机磷农药的残留方法

了解当前本市农产品市场中关于蔬菜中有机磷农药残留的相关状况,制定相关对策,建立一种适用于多种有机磷农药快速检测的气相色谱方法。根据农药的相关性质,该气相色谱法可同时检测15种有机磷农药,其中包括:敌百虫、敌敌畏、甲胺磷、乙酰甲胺磷、灭线磷、甲拌磷、氧乐果、特丁硫磷、乐果、甲基对硫磷、马拉硫磷、杀螟硫磷、对硫磷、倍硫磷、水胺硫磷。通过对不同型号色谱柱的选择、柱温箱升温程序的控制,实现对15种常见有机磷农药的快速、便捷、准确度好的定性和定量的分析。     

固相萃取-GC-MS法检测铁皮石斛药材中的5种常见农药残留

目的建立固相萃取-气相色谱-质谱法(GC-MS)测定铁皮石斛中5种有机磷农药残留量的分析方法。方法样品用乙腈匀浆提取,氯化钠盐析后,提取液经氨基固相萃取柱净化,GC-MS分析测定,内标法定量。结果 5种有机磷农药呈良好的线性关系(相关系数r0.995),线性范围为0.01～2.0μg/ml,检出限为:甲基对硫磷0.006 mg/kg,杀螟硫磷0.006 mg/kg,马拉硫磷0.003 mg/kg,对硫磷0.006 mg/kg,杀扑磷0.001 mg/kg。6次进样RSD小于5%,回收率为85.1%～96.5%。结论该方法具有操作简单、重现性好、速度快等优点,可用于测定铁皮石斛中微量有机磷农药残留量。     

气相色谱法测定粮食中4种有机磷农药残留量的不确定度评定

目的 对气相色谱法测定粮食中乐果、杀螟硫磷、对硫磷、马拉硫磷农药残留量的方法进行不确定度评估。方法 依据JJF 1059.1-2012《测量不确定度评定与表示》和JJF 1135-2005《化学分析测量不确定度评定》中有关规定, 建立了用气相色谱法测定粮食中4种有机磷农药残留量的不确定度评估数学模型, 对测定中的不确定度来源进行分析和评估。结果 当粮食中乐果、杀螟硫磷、对硫磷、马拉硫磷的残留量分别为0.10、0.19、0.095、0.093 mg/kg时, 扩展不确定度分别为: 0.01、0.01、0.010、0.006 mg/kg, 4种有机磷残留量分别表示为: (0.10±0.01) mg/kg (k=2)、(0.19±0.02) (k=2)、(0.095±0.006) mg/kg (k=2)、(0.093±0.007) mg/kg (k=2)。 结论 实验过程中的不确定度主要来源于标准物质配制和样品稀释过程, 本评估方法可为气相色谱法检测多组分农药残留量的不确定度评估提供依据。     

茶叶中有机磷农药残留测定方法的改进

茶叶是我国一种重要的出口经济作物,我国的茶叶产量居首位,茶叶的质量对于保障人类健康、促进我国经济增长具有重要作用,但近些年来,茶叶中残留农药问题造成的茶叶质量不合格问题时有发生。基于此,文章建立了一种简便快速测定方法,能够对茶叶中残留的七种有机磷农药敌敌畏、乐果、毒死蜱、甲基对硫磷、马拉硫磷、杀螟硫磷、三唑磷进行测定,以期为茶叶中有机磷农药残留测定方法的改良提供理论支持。     

Survey of organophosphorus pesticide residues in virgin olive oils produced in Chile

Dimethoate, diazinon, parathion methyl, pirimiphos methyl, malathion, fenthion, chlorpyriphos, methidathion and azinphos methyl were determined in 71 olive oil samples produced in Chile from different varieties of olives (arbequina, frantoio, picual, lechino and blend) at three different harvest periods (2007, 2008 and 2009). The target pesticides were determined using a validated analytical method based on microwave-assisted liquid–liquid and solid-phase extraction with subsequent GC–FPD detection and GC–MS/MS for confirmation purposes. In 79% of the samples, five of the nine pesticides tested were detected with a frequency of one pesticide per sample. The highest detection rates were observed for the residues of chlorpyriphos and diazinon. The average concentration of chlorpyriphos, diazinon, azinphos methyl and methidathion were 0.084, 0.057, 0.024 and 0.010 µg g^?1, respectively. Higher contents of organophosphorus pesticides (OPPs) were found in regions where intensive agriculture is practiced. However, the levels of OPPs were reassuringly low and indicate that olive oil produced and exported from Chile does not currently represent any risk for consumers.     

Survey of pesticide residues in imported cereal products (1994.4 approximately 2006.3)

A survey of pesticide residues in 490 imported cereal products on the Tokyo market from April 1994 to March 2006 was carried out. Eight kinds of organophosphorus pesticides (chlorpyrifos, chlorpyrifos-methyl, DDVP, diazinon, etrimfos, malathion, MEP and pirimiphos-methyl) were detected at levels between Tr (below 0.01 ppm) and 0.82 ppm from 91 samples.In our investigations, chlorpyrifos-methyl and malathion tended to be detected in samples from America, pirimiphos-methyl in those from Europe, and MEP in those from Oceania. Thus, pesticide residues seemed to be different in produce from different areas.Residue levels of these pesticides were calculated as between 0.08 and 13.2% of their ADI values according to the daily intake of cereal products. Therefore, these cereal products should be safe for normal usage.     

烟草中抑芽丹残留量的测定

采用ISO 4876-1980规定的方法测定了239个国产烟叶、49个进口烟叶和12个进口卷烟样品中的抑芽丹残留量。结果表明:国产烟叶抑芽丹的检出率为6.69%,最高54.00mg/kg,最低1.50mg/kg,平均6.82mg/kg;进口卷烟检出率为58.33%,最高42.75mg/kg,最低7.75mg/kg,平均17.57mg/kg;进口烟叶检出率为30.61%,最高14.00mg/kg,最低1.50mg/kg,平均5.63mg/kg。     

Analysis of pesticide residues in bananas harvested in the Canary Islands (Spain)

In this work, 11 pesticides (ethoprofos, dimethoate, diazinon, malaoxon, chlorpyrifos-methyl, fenitrothion, malathion, chlorpyrifos, fenamiphos, buprofezin and phosmet) were analysed in 57 banana samples taken from the local markets of the Canary Islands (Spain). Analyses were carried out by the QuEChERS approach developed for pesticide residue analysis in food, using gas chromatography (GC) with nitrogen–phosphorus detection (NPD). Triphenylphosphate (TPP) was used as internal standard. Recoveries ranged between 67% and 118% with RSD values below 16%. Typical limits of quantification (LOQs) of the method were 0.01–0.14 mg/kg, which are below the EU maximum residue limits (MRLs) established for these compounds in bananas. Chlorpyrifos was detected in 50 samples (88%) in the concentration range 0.03–0.65 mg/kg, malathion in five samples (8.8%) in the concentration range 0.16–0.17 mg/kg, fenitrothion in four samples (7.0%) in the concentration range 0.02–0.10 mg/kg and buprofezin in one sample (1.8%) at 0.15 mg/kg. All these values are below the MRLs established for these compounds except for two samples containing fenitrothion. Among the studied pesticides only chlorpyrifos has a high occurrence in the samples. However, the levels of these residues cannot be considered a serious public health problem according to EU regulations. Because of the high occurrence of chlorpyrifos, its distribution between the pulp and the peel was also investigated. Results show that most of the pesticide remains in the peel and that only amounts between 0.07 and 0.12 mg/kg occur in the pulp even at concentrations in the peel as high as 0.87 mg/kg.     

Decay of dinitroaniline herbicides and organophosphorus insecticides during brewing of lager beer

This article examines the fate of four pesticides that can be present during the brewing of lager beer. For this purpose, malted barley was spiked at 2 mg/kg with pendimethalin and trifluralin (dinitroaniline herbicides) and fenitrothion and malathion (organophosphorus insecticides). Analyses of pesticide residues were carried out by a gas chromatograph with an electron capture detector, and their identity was confirmed by gas chromatography-mass spectrometry. Cleanup was necessary for the malt and spent grain samples. Beginning with mashing and ending with the final product 4 months later, various samples (spent grain, sweet wort, brewer wort, and beer) were taken to determine the concentration of the targeted residual pesticides during the various beer making phases. In all cases, the residual levels recorded in sweet wort sampled after the mashing phase were below the respective maximum residue limits established by Spanish legislation for barley. Significant proportions of pesticide residues (17 to 40%) were retained on the spent grain. Applying the standard first-order kinetics equation (r > 0.91), the half-lives obtained for the four compounds during the storage of the spent grain (3.5 months) varied from 138 days (fenitrothion) to 192 days (malathion and pendimethalin). Herbicide residues practically disappeared (<0.3%) after wort boiling, whereas the percentages of the remaining insecticides, fenitrothion and malathion, ranged from 3.5 to 4.3%, respectively, at this time. No residues of dinitroaniline compounds were detected in young beer, whereas there was a significant reduction in fenitrothion (58%) and malathion (71%) residues during fermentation. Lagering and filtering processes also reduced the content of the organophosphorus insecticides (33 to 37%). Finally, after the storage period (3 months), the content of fenitrothion was reduced by 75%, with malathion residues being below its detection limit.     

Insecticides extraction from banana leaves using a modified QuEChERS method

An analytical method employing gas chromatography (GC) with nitrogen–phosphorus detection has been developed for the simultaneous determination of eight insecticides (seven organophosphorus pesticides: ethoprophos, diazinon, chlorpyrifos-methyl, fenitrothion, malathion, chlorpyrifos and fenamiphos, and one thiadiazine: buprofezin) in banana leaves that are currently being used to feed cattle or hogs. The extraction and preconcentration of these pesticides were carried out using a modified QuEChERS procedure and the whole method was validated in terms of repeatability, linearity, precision and accuracy. Triphenylphosphate was used as internal standard. Matrix effect evaluation was also carried out using a matrix matched calibration. The developed procedure gave satisfactory recovery (89–104%) and relative standard deviation values (<9.1%) for the studied pesticides in banana leaves, while limits of detection ranged between 0.002 and 0.064 mg/kg. The method was finally applied to the determination of these pesticides in 12 treated banana leaves samples collected at different banana cultivars of the Canary Islands. Residues of chlorpyrifos were found in ten of these samples. Pesticide confirmation was carried out by GC with tandem mass spectrometry detection.     

Organophosphorus pesticides residues in Italian raw milk

Organophosphorus pesticides (OPPs), widely used in agriculture, can cause toxic effects to humans and animals. The main purpose of the present work was to determine the contamination in raw milk by the main organophosphorus pesticides used in Italy and to evaluate the opportunity to start specific procedures of risk management along the milk production chain. The samples, collected in 4 Italian dairy plants directly from the tank trucks during the delivering, were representative of 920 tonnes of raw milk. The isolation of the OPPs (acephate, chlorpyriphos, chlorpyriphos-methyl, diazinon, methamidophos, methidathion, phorate, pirimiphos-methyl) was performed by liquid partition followed by clean-up with solid phase extraction. The analyses were carried out by dual column gas chromatography using two nitrogen-phosphorus detectors. Among the 135 samples analysed, 37 were positive in traces and 10 showed an OPP contamination ranging from 5 to 18 microg/kg. The higher results were recorded in the samples collected during the autumn-winter period. The main pollutants detected were acephate and chlorpyriphos. In every positive sample found, the OPP contamination was lower than the maximum residue level (MRL) fixed by the European Commission.     

烟草中游离氨基酸的自动分析仪测定

以茚三酮为显色剂(溶液流速:0.30mL/min),柠檬酸钠水溶液为缓冲液(流速:0.45/min),在柱温53℃、反应温度138℃及570nm和440nm检测波长下利用氨基酸自动分析仪测定了国产和进口18种白肋烟烟叶和11种混合型卷烟中的游离氨基酸含量。结果表明:①进口白肋烟烟叶的游离氨基酸总量明显高于国产烟叶;②进口白肋烟中的天冬氨酸、谷氨酸含量高于国产烟叶,而国产白肋烟中的脯氨酸含量高于进口烟叶;③进口混合型卷烟的游离氨基酸总量明显高于国产卷烟,尤其是天冬氨酸、白氨酸、酪氨酸和脯氨酸。     

进口烤烟与我国主产区烤烟烟叶物理特性相似性分析

为明确进口烤烟烟叶与国产烟叶物理特性的相似性,对比分析了津巴布韦、赞比亚、马拉维和坦桑尼亚4个国家不同等级进口烤烟烟叶物理特性,并与我国云南、贵州等11个主产区烤烟烟叶物理特性进行聚类分析。结果表明：（1）我国烟叶叶面密度、厚度、平衡含水量和填充值与进口烟叶接近,拉力高于进口烟叶,单叶质量低于进口烟叶。（2）山东、四川、重庆、云南等地烤烟烟叶物理特性与进口烟叶较为接近,与马拉维和坦桑尼亚烤烟烟叶相似性较高,与津巴布韦和赞比亚烟叶相似性略次。广东、湖北、贵州、湖南、福建、河南、陕西等地烟叶与进口烟叶物理特性差异较大。