Investigation of pesticide residues in vegetables and fruits grown in various regions of Hatay,Turkey

In this study, 175 pesticide residues in various vegetable and fruit samples grown in different regions of Hatay, Turkey, were investigated. Residue analyses were performed using liquid chromatography–tandem mass spectrometry with the QuEChERS method. In tomato, plum and apricot samples, pesticide residues were below the limits of detection. In other samples, at least one pesticide residue was detected. Twelve pesticides (acetamiprid, carbendazim, chlorpyrifos, fenarimol, fludioxonil, hexythiazox, imidacloprid, metalaxyl, pyridaben, pyriproxyfen, thiabendozole, triadimenol) were found at levels between 0.003 and 0.759?mg?kg^?1. Only in cucumber samples, acetamiprid residues were found at levels greater than the maximum acceptable limit in Turkish Food Codex and European Union maximum residue limits (EU MRLs). In other samples, the detected residue amounts are less than the MRLs declared in the Turkish Food Codex and EU MRLs.     

Pesticide residues in fruits and vegetables in Jordan using liquid chromatography/tandem mass spectrometry

A total of 158 fruit and vegetable samples produced in Jordan were examined for the presence of pesticide residues using the multi-residue analysis technique by Liquid Chromatography-tandem Mass Spectrometry (LC-MS/MS) and the QuEchERS extraction method. A total of 73 samples (46%) were free from detectable residues, while 85 samples (54%) contained residues. Among the tested samples, 34 (22%) contained residues above Maximum Residue Levels (MRLs) and 51 (32%) contained residues at or below MRLs. Most of the detected residues were found in sweet pepper, peach and apricot samples. Only watermelon samples were free from detectable residues, while tomato and melon samples exhibited residues below MRLs. Out of the 113 pesticides tested, 22 pesticides were found above the limit of detection, 9 of which (hexaconazole, propargite, propiconazole, myclobutanil, thiamethoxam, thiacloprid, clothianidin, clofentezine and pyridaben) had residues that violate MRLs according to European regulations. A continuous monitoring programme for pesticide residues in Jordanian fruits and vegetables is highly recommended.     

Pesticide residues determination in China vegetables in 2010–2013 applying gas chromatography with mass spectrometry

The levels of multi-pesticide residues in highly consumed types of vegetables in western regions of China were investigated in this study. Vegetable samples (506) were collected from local markets from 2010 to 2013, and the concentrations of 21 types of organophosphorus (OP) and pyrethroid (PYR) pesticides from the samples were determined by gas chromatography–mass spectrometry (GC–MS). Ten OP pesticides were found in concentrations ranging from 0.0008 to 4.0544 mg/kg. Five types of PYR pesticides were determined to have concentrations in the range of 0.0009 to 6.0827 mg/kg. There were no residues in 69.76% of the samples. A portion (25.49%) of the samples contained pesticide residues less than or equal to the maximum residue limits (MRLs), and 4.94% of samples contained pesticide residues greater than their MRLs. This study provides useful information on the current contamination status of a key agricultural area in China from 2010 to 2013 and highlights the need for regular monitoring of pesticide residues in a greater number of vegetable samples and for longer periods, especially in leafy vegetables, to protect consumers.     

国内外大蒜农药残留限量对比分析

目的 掌握国内外大蒜中农药最大残留限量(Maximum residue limits,MRLs)标准现状,以便降低大蒜出口贸易风险,并在此基础上对完善我国大蒜农残限量标准提出建议。方法 收集我国与欧盟、国际食品法典委员会(Codex Alimentarius Commission, CAC)、日本和韩国等5个组织或国家的大蒜农药MRLs标准并进行对比分析。 结果 我国大蒜农药MRLs标准有129项,欧盟、日本、韩国和CAC分别有510、252、173和23项。欧盟、日本、韩国和CAC标准中与我国相同的农药种类数量分别有93、67、56和18项,其中限量值低于中国标准的分别占49、19、22和4项。结论 由于各国膳食结构不同及登记使用的农药情况不同,我国与欧盟、CAC、日本和韩国大蒜MRLs标准指标总数及指标要求差异明显,建议结合我国大蒜生产实际及膳食需求,完善我国相关标准。     

Pesticide residues survey in citrus fruits

The use of pesticides is widespread in citrus fruits production for pre- and post-harvest protection and many chemical substances may be applied in order to control undesirable moulds or insects. A survey was carried out to evaluate levels of pesticide residues in citrus fruits. Two multiresidue analytical methods were used to screen samples for more than 200 different fungicides, insecticides and acaricides. A total of 240 samples of citrus fruits including lemon, orange, mandarin, grapefruit, lime, pomelo and kumquat were taken in various markets in the Geneva area during the year 2003. Ninety-five percent of the 164 samples issued from classical agriculture contained pesticides and 38 different compounds have been identified. This high percentage of positive samples was mainly due to the presence of two post-harvest fungicides, imazalil and thiabendazole, detected in 70% and 36% of samples respectively. Only three samples exceeded the Swiss maximum residue limits (MRLs). Fifty-three samples sold with the written indication “without post-harvest treatment” were also controlled. Among theses samples, three exceeded the Swiss MRLs for penconazole or chlorpyrifos and 18 (34%) did not respect the written indication since we found large amounts of post-harvest fungicides. Finally, 23 samples coming from certified organic production were analysed. Among theses samples, three contained small amounts of pesticides and the others were pesticides free.     

Residue levels and health risk of pesticide residues in bell pepper in Shandong

ABSTRACT

The purpose of this study was to investigate pesticide residues in bell peppers from Shandong Province, China. A total of 299 samples were collected from 17 cities in 2016. The concentrations of 26 pesticide residues were determined by gas chromatography with mass spectrometry (GC–MS). The results showed that there were 25 pesticides (15 OPs, 7 PYs, 3 CBs) found in 86 bell pepper samples, and the total number of positives was 120. The total frequency was 28.76%. The detection frequency for OPs, PYs and CBs was 16.39%, 12.37% and 3.01%, respectively. The most frequently detected pesticide was bifenthrin, with the frequency of 5.02%. 5.35% of samples contained pesticide residues above the maximum residue limits (MRLs) set by China. 7.36% of samples contained more than one pesticide. The values of %ADI were below 100, while the %ARfD of carbofuran and methidathion exceeded 100 for children. The cumulative risk was highest for OPs. From the public health point of view, the levels of pesticide residues in bell peppers do not pose a serious health risk to adults, but the acute health risk to children should be paid more attention.     

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.     

甜瓜MRLs增补种类及其建议值分析

为明确甜瓜最大残留限量值增补种类及其建议值,本文以2018和2019年6个省份545份甜瓜为实验材料,在完成实验材料中60种农药残留定量分析的基础上,通过急性膳食风险分析(％ADI)、慢性膳食风险分析(％ARfD)、风险矩阵等技术方法,探讨了甜瓜残留农药的质量安全风险,开展了风险相对较高残留农药及最大残留限量值(MRL...     

我国主产地柑橘的农药残留现状研究

我国柑橘生产使用农药种类多、剂量大,对产品质量安全有一定影响。文中采用气相色谱和高效液相色谱检测技术,对我国6省(市)柑橘产地抽取的198个鲜果样品进行了26种农药残留的检测与评价。10种农药残留检出,包括禁限用农药,其中1个样品有1种农残超标,超标率为0.47%,各省(市)柑橘鲜果样品的农药残留检出率均在48.9%以上,我国柑橘质量安全存在潜在风险。     

A multi-residue method for the determination of pesticides in high water content matrices by gas chromatography-single quadrupole mass spectrometry with electron ionisation (EI-GC/MS)

An EI-GC/MS method for the determination of pesticide residues in vegetable matrices with high water content was validated using papaya samples. The validation of a multi-residue pesticide method was in agreement with national and international regulations enabling the Ministry of the Agriculture, Livestock and Food Supply of Brazil to cover a large number of matrices and pesticide residues in its monitoring and control programmes. The extraction used 60 mL of ethyl acetate and 30 g of sample previously processed. After extraction, clean-up of all the extracts was carried out by percolation through GBC cartridges. The samples were then injected in an EI-GC/MS system. Calibration curves were prepared in quadruplet by fortifying blank extracts with a standard solution containing all the pesticides studied at 0.000, 0.005, 0.010, 0.020, 0.030, 0.050, 0.080 and 0.100 mg kg(-1). For the recovery study, blank samples were fortified at 0.010, 0.020, 0.030, 0.050 and 0.080 mg kg(-1) and then submitted to the extraction procedure. The complete procedure was repeated over four different days by two analysts. The regression parameters of calibration curves were calculated for each validation day. Linearity, selectivity, specificity, robustness, limits of detection and quantification were also assessed. The uncertainty was estimated for each analyte at each spike level studied. The method had recoveries between 91% and 105% and precision results ≤ 20%. Limits of quantification were below or equal to the maximum residue limits (MRLs) regulated by Brazilian legislation. The MRLs of the selected pesticides are not regulated by CODEX Alimentarius. The results are also in agreement with SANCO/10684/2009.     

河北产区桃农药残留风险评估

目的 明确河北产区桃中农药残留水平和风险状况。方法 在河北省采集70份桃样品进行农药残留检测与分析,对检出农药残留行急性和慢性膳食摄入风险评估,并利用风险排序矩阵对农药残留风险大小进行排序。结果 70批次桃样品共检出农药残留33种,农药残留检出率为100%,个别样品存在农药残留超标现象,超标农药为多菌灵和甲氨基阿维菌素苯甲酸盐。桃中检出农药的慢性膳食摄入风险(%ADI)在0.00%～1.06%之间,急性膳食摄入风险(%ARfD )在0.00%～11.34%之间。根据农药残留风险排序结果,高风险农药共有5种,其中毒死蜱和甲氨基阿维菌素苯甲酸盐检出率较高,分别为45.7%和18.6%。结论 河北地区桃样品中农药残留检出率较高,但94.3%的样品中农药残留量符合国家限量标准,桃中农药残留急性和慢性膳食摄入风险均处于较低水平,其中,多菌灵、毒死蜱和甲氨基阿维菌素苯甲酸盐是桃中应重点关注的风险因子。     

2012—2014年青岛、深圳、大连三口岸282份进口水果和蔬菜中农药残留监测

目的掌握和了解进口水果和蔬菜中农药残留污染状况,为国家制定和完善相关标准和采取相关措施提供科学依据。方法本文采用GB/T 19648—2006《水果和蔬菜中500种农药及相关化学品残留量的测定气相色谱-质谱法》和GB/T 20769—2008《水果和蔬菜中450种农药及相关化学品残留量的测定液相色谱-串联质谱法》分析方法,对2012—2014年从青岛、深圳、大连三个主要水果和蔬菜进口口岸采集的282份水果和蔬菜样品进行了666种农药残留的检测。结果对282份水果和蔬菜样品进行农药残留测定和技术分析:未检出农药残留样品31份,占11.0%;检出农药残留样品251份,占89.0%。共检测出农药52种,频次702次。结合中国、欧盟、日本的农药最大残留限量标准,对获得的数据进行了科学的分析:进口香蕉、榴莲、火龙果、草莓的农药残留水平整体处于安全水平,应加强进口龙眼、樱桃、葡萄中农药残留的检测和监管。结论进口水果和蔬菜的农药残留检出率较高,达到89.0%,但超出中国最大残留限量标准的样品较少,只占1.1%,说明进口水果和蔬菜中农药残留整体处于安全水平。     

国内外枸杞农药残留限量标准对比分析

目的 对比不同国家、地区枸杞中农药的最大残留限量(maximum residues limits, MRLs)标准, 对其差异进行分析。方法 查阅整理我国、欧盟、国际食品法典委员会(Codex Alimentarius Commission, CAC)、韩国和日本关于枸杞农药MRLs的标准, 分析我国、欧盟、CAC、韩国和日本在枸杞农药MRLs标准体系上的差异。结果 我国规定了枸杞中116种农药MRLs标准, 而欧盟、CAC、韩国、日本分别规定了498、15、53、214种标准, 我国标准与欧盟、CAC、韩国和日本的标准共同关注度分别是13.9%、11.0%、5.7%和17.4。结论 我国对比欧盟、CAC、韩国及日本的枸杞农药MRLs标准中种类及数量均存在差异,但我国标准符合我国实际国情。为了避免枸杞出口受阻, 在修订我国枸杞农药MRLs标准时, 可以参考与我国有枸杞贸易往来的其他国家、地区及组织的标准。     

芦笋中农药最大残留限量及检测方法研究进展

总结了芦笋中常用农药及欧盟、日本、美国和我国对其最大残留限量规定,并对农药残留相关检测方法在芦笋等果蔬中的应用进行综述,以期为我国芦笋中农药残留检测和控制提供参考。     

杨桃中化学污染物分析及农药残留暴露评估

以杨桃为研究对象,对广东、广西、海南和福建的基地收购点、批发市场和农贸市场等地点的样品进行化学污染物残留分析。结果表明：农贸市场和水果摊样品的农药残留种类少,基地收购点的农残种类最多,超标样品集中在基地收购点。检出率最高的3 种农药为氯氰菊酯、多菌灵和灭幼脲。3 份样品检出镉超标。经点评估对农药残留初步分析,杨桃中的残留风险总体较低,仅三氯杀螨醇存在潜在风险。分布点评估的结果表明,在较高的置信概率P99.5风险水平下,三氯杀螨醇暴露量在幼儿和儿童（2～10 岁）的亚群超过日允许摄入量,存在不可接受的风险。建议重点对基地收购点样品监控,制定三氯杀螨醇、多菌灵和灭幼脲在杨桃上的最大残留限量或筛选三氯杀螨醇的替代品。     

Pesticide residues in grapes from vineyards included in integrated pest management in Slovenia

Although the list of pesticides used in integrated pest management (IPM) in grape growing and their annual application rates are limited, we are still confronted with the problem of pesticide residues in grapes. This paper presents the results of pesticide monitoring of 47 samples of wine grapes (Vitis vinifera L.) from the 2006 vintage from vineyards included in IPM. The grape samples were analysed for the presence of 67 pesticides. Among them 20 were allowed in IPM in 2006. Grapes were sampled at harvest. Two internal analytical methods were used for the determination of pesticides: gas chromatography-mass spectrometry (GC-MS) method for the determination of dithiocarbamates and a multi-residue GC-MS method. One grape sample (2.1%) contained no residues or they were below the limit of detection, 28 samples (59.6%) contained residues lower or equal than maximum residue levels (MRLs), and 18 samples (38.3%) exceeded national MRLs for cyprodinil (the concentration range was 0.03–0.40 mg kg^?1 of cyprodinil) and fludioxonil (concentration was 0.03 mg kg^?1 of fludioxonil). Multiple residues were found in 41 samples (87.2%). The highest number of pesticides detected per sample was seven. No violation of pesticides allowed in IPM was observed. Folpet (97.9%), cyprodinil (51.1%), dithiocarbamates (44.7%), chlorothalonil (23.4%), chlorpyriphos (19.1%) and pyrimethanil (14.9%) were the most frequently found pesticides in grapes. Risk assessment showed that the exceeded concentrations of cyprodinil and fludioxonil did not represent any risk for consumer's health (the national estimate of short-term intake as a percentage of the acceptable daily intake was below 100%).     

北方地区枣果农药残留风险评估

目的围绕我国北方地区枣果农药残留问题,开展膳食暴露风险评估研究。方法采集北方地区枣果主产省份(河北、山东、河南、陕西和山西)的102份枣果样品,对82种常用农药和23种禁限用农药进行检测,分别利用急性参考剂量(ARf D)和每日允许摄入量(ADI)进行急性和慢性膳食暴露风险评估,并利用风险排序矩阵对检出农药进行风险大小的排序。结果 102份样品中89份样品检出了农药残留,共检出37种农药,其中2个样品检出农药残留超标,超标农药分别为多菌灵和氰戊菊酯。枣果中检出农药的急性膳食暴露风险(用%ARf D表示)介于0.00%~6.01%之间,平均值为1.82%;慢性膳食暴露风险(用%ADI表示)介于0.00%~0.21%之间,平均值为0.03%。根据农药残留风险得分,检出残留的37种农药可划分为4类,即高风险农药(2种)、中风险农药(3种)、低风险农药(13种)和极低风险农药(19种)。结论我国北方地区枣果中农药残留检出率较高,98%的样品农药残留量符合国家限量标准,枣果中农药急性膳食和慢性膳食暴露风险均处于较低水平,地虫硫磷、克百威、毒死蜱、联苯菊酯和唑螨酯是枣果中应重点关注的农药风险因子。     

2018年欧盟食品中农药残留情况分析及启示

欧盟向来十分重视食品安全, 在农药残留监管方面, 建立了健全的农药残留监管体系。 本文从欧盟农药残留法规标准、监管部门及分工和欧盟农药残留控制计划3方面介绍了欧盟农药残留监管体系, 从欧盟协调控制计划和国家控制计划两部分分析了2018年欧盟食品中农药残留情况, 涉及样品来源、产品、农药、食品中草甘膦、进口食品、婴幼儿食品、有机食品和动物源性食品等。本文也指出了农药残留产生的原因和风险评估结果, 提出风险管理建议, 并借鉴其监管思路, 提出对我国农药残留监管的几点建议, 为食品安全监管决策提供参考。     

Pesticide residues in leafy vegetables,stalk and stem vegetables from South Korea: a long-term study on safety and health risk assessment

South Korea has a unique food culture. South Koreans enjoy wrapping meat and eating or making kimchi (traditionally fermented Korean food) and eating using raw leafy vegetables, stalk and stem vegetables. Therefore, there is a high chance of being exposed to pesticide residues of vegetables. The objective of this study was to investigate pesticide residues in leafy vegetables, stalk and stem vegetables from South Korea. A total of 8496 samples were mainly collected from Gwangju and Jeonnam area (the largest production region of leafy vegetables, stalk and stem vegetables) in South Korea from 2010 to 2014. A total of 230 pesticides were used for multi-residue analysis of pesticides. Among 8496 samples, 61 different pesticides (1029 times) were detected in 890 samples, of which 118 samples (1.4%) exceeded the Korea maximum residue limits (MRLs). Samples exceeding the MRLs were mostly found in leafy vegetables (brassica lee ssp. namai, leafy lettuce, spinach, perilla leaves, crown daisy, marsh mallow, aster scaber, pimpinella brachycarpa) and Chinese chive. Procymidone, dimethomorph and azoxystrobin were the most frequently found pesticides. A risk assessment of pesticides exceeding the MRLs was evaluated by calculating the estimated daily intake (EDI) and the acceptable daily intake (ADI). The ratio of EDI to ADI was 0.003–30.4%.     

Effects of processing and cooking on the levels of pesticide residues in rice samples

The effects of processing and cooking on the levels of pesticide residues in rice samples were investigated for 11 pesticides in pre-harvest (9 pesticides) and post-harvest (4 pesticides) samples. In the polishing process, the transfer ratio (%, total pesticide residue amount in product/that in brown rice) of rice bran ranged from 40% to 106%, and the transfer ratio of polished rice ranged from 9% to 65% in pre-harvest samples. These values varied from pesticide to pesticide. The processing factor (the concentration (mg/kg) of pesticide in product/that in the brown rice) of polished rice ranged from 0.11 to 0.73. The loss of pesticides during processing and/or cooking did not correlate to any single physical or chemical property. Investigation of changes of pesticide residues during processing and/or cooking is useful not only to establish MRLs, but also to recognize actual levels of pesticide residues in food.