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。     

Study of pesticide residues in agricultural products for the "Positive List" system

During a 3-year monitoring survey (April 2002-March 2005) of pesticide residues in agricultural products, 592 samples (324 domestic; 268 imported) collected in Hyogo prefecture, Japan were analyzed. The number of pesticides tested increased from 232 in FY 2002 to 323 in FY 2004. The purpose of the study was to clarify the residue status by accumulating information about pesticides detected frequently, to allow effective and efficient regulation under the new "Positive List" legislation to be implemented in FY 2006. Overall, 47% of domestic and 61% of imported samples contained detectable residues and ca. 60% of positive samples contained multiple residues. The limit of quantitation was set at 0.01 microg/g and the limit of detection was 0.001-0.003 microg/ g. Most of the residues were present at low concentrations: 80% of the detections in samples excluding imported citrus fruits were < 0.05 microg/g. More than 5 different pesticides (> 0.01 microg/g) were detected simultaneously in 13 samples. The sum of the ratios of residues to MRLs was calculated as one of the indexes to represent the risk of multiple residues, and they exceeded 100% in 3 imported frozen vegetables; baby kidney bean, spinach, Welsh onion. Samples in violation of the Food Sanitation Law were not found in our survey, but 1.9% of the samples might be in conflict with the new "Positive List" legislation.     

Monitoring of pesticide residues in Egyptian fruits and vegetables during 1997

A total of 2318 domestic samples of different types of fruits and vegetables were collected from eight Egyptian local markets in six different regions of the country. All samples were examined for residues of 54 pesticides, including organophosphorus, organonitrogen, organohalogen and certain pyrethroides. However, dithiocarbamates were analysed in only 318 samples. Overall, 81.5% of the samples had no detectable pesticide residues. Of the contaminated samples, 18.5% contained detectable residues and 1.9% exceeded their maximum residue limits (MRLs). Root and leafy vegetables showed the lowest contamination rates (1.9 and 4.7%, respectively), slightly exceeding the MRLs in leafy vegetables. However, fruit samples showed a slightly higher proportion of contamination than vegetables (29 and 14.3%, respectively). Fruit also exhibited a higher level of violation than vegetables (2.3 and 1.9%, respectively). The contamination and violation rates were lower than the percentages recorded in previous years' monitoring studies. Dicofol and dimethoate were the most frequently occurring pesticide residues at 5.1 and 5.0%, respectively. Dimethoate showed higher violation levels (0.69%). However, dicofol showed a slight violation rate (0.09%) which indicates good agricultural practices for dicofol use. Dithiocarbamates residues were found in 21 of the 318 samples analysed, which when expressed as a percentage contamination was 6.6%, and only one sample exceeded the MRL.     

Investigation of pesticide residues in foods distributed in Kitakyushu City

We investigated 160 kinds of pesticide residues in 715 samples of 116 kinds of foods distributed in Kitakyushu city. Sixty kinds of pesticides were detected in 55 kinds of foods (204 samples) in the range of 0.002-22 mg/kg. Five kinds of pesticides in 7 samples violated the residue standards and the indication of "unused". The detection ratios of unregulated pesticide in domestic and imported foods were 27.8 and 33.0%, respectively. Iprodione, dicofol, diethofencarb, procymidone and chlorfenapyr (for domestic food) and total bromine, benomyl, chlorpyrifos, dicofol, fenvalerate, cypermethrin and dimethoate (for imported food) showed relatively high detection ratios. Chinese cabbage, garland chrysanthemum, tomatoes and green teas (domestic) and broccoli, bananas, grapefruit, lemons, oranges, frozen edamame and frozen kidney beans (imported) showed high relative pesticide detection ratios. Residual pesticides were detected with relatively high frequency in imported fruits, imported frozen foods and imported processed foods.     

Organophosphorus pesticide residues in market foods in Shaanxi area,China

The aim of this study was to investigate the organophosphorus (OP) pesticide residues in market foods (cereals, vegetables, and fruits) in the Shaanxi area of China. The concentrations of eight OP pesticides were determined by gas chromatography with flame photometric detection (GC-FPD). In 18 of 200 samples, five OP pesticides, including dichlorvos, dimethoate, parathion-methyl, pirimiphos-methyl and parathion, were found in concentrations ranging from 0.004 to 0.257 mg/kg. The mean levels of dimethoate in fruits and parathion in vegetables exceeded the maximum residue limits (MRLs) allowed by the Ministry of Health, of China. Other detectable OP pesticide residues levels were below their MRLs. Demeton, diazinon and sumithion were not found in any sample. The results provide important information on the current contamination status of a key agricultural area in China, and point to the need for urgent action to control the use of some excessively applied and potentially persistent OP pesticides, such as dimethoate and parathion.     

北京市蔬菜、水果中有机磷农药残留现状调查

为了解北京市蔬菜、水果中有机磷农药残留情况，2002年在北京市抽检样品354件进行13种有机磷监测，其中蔬菜28l件，水果73件。检测结果显示7．6％的检品不符合国家标准。叶菜类(14，占9．3％)和根茎类(8，占17．4％)蔬菜的不合格率明显高于瓜菜、果菜类(2，占2．4％)蔬菜和水果(3，占4．1％)。13种有机磷检测出12种，其中禁用农药占53％。本市种植的蔬菜、水果与外埠进京产品的有机磷农药残留情况无显差别，超市、集贸市场、批发市场销售的产品的不合格率亦无显差别。     

Evaluation of pesticide residues in fruits and vegetables from Algeria

ABSTRACT

A total of 160 samples of 13 types of fresh fruits and vegetables from domestic production and import were analysed to detect the presence of pesticide residues. Analysis was performed by multi-residual extraction followed by gas chromatography–mass spectrometry. In 42.5% of the tested samples, no residues were found and 12.5% of samples contained pesticide residues above maximum residue limits. Risk assessment for long-term exposure was done for all pesticides detected in this study. Except chlorpyrifos and lambda-cyhalothrin, exposure to pesticides from vegetables and fruits was below 1% of the acceptable daily intake. Short-term exposure assessment revealed that in seven pesticide/commodity combinations, including three pesticides (chlorpyrifos, deltamethrin and lambda-cyhalothrin), the acute reference dose had been exceeded.     

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.     

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 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%.     

苏南某市叶类蔬菜含氯有机农药残留状况分析及风险评估

目的了解苏南某市叶类蔬菜中含氯有机农药的残留状况及其质量安全现状。方法利用气相色谱法对采集自该市农贸市场、大型超市、种植基地及散户的6种主要叶类蔬菜中5种代表性的含氯有机农药(百菌清、三唑酮、氟氯氰菊酯、氯氰菊酯和氰戊菊酯)进行定量检测分析,采用食品安全指数开展暴露风险评估。结果 5种含氯有机农药在蔬菜样本中均有不同程度的检出,平均检出率为13.8%,百菌清、氯氰菊酯2种农药在部分蔬菜样本中的残留超标,超标率分别为0.4%和0.9%。6种叶类蔬菜的农药安全指数平均值均小于1,说明被检蔬菜的安全状态可为消费者所接受。但百菌清在菠菜和生菜中的安全指数均大于1,表明百菌清对菠菜和生菜质量安全的影响风险超过了可接受的限度。结论该地区主要叶类蔬菜的整体质量较安全,被检农药的残留状况总体良好,但对菠菜和生菜生产中百菌清的使用需加大监督管理力度,确保消费者食用蔬菜的安全性。     

2012~2016年杭州市富阳区蔬菜中农药残留 监测及分析

目的 了解我国南方地区蔬菜中农药残留情况,为制定蔬菜农药残留限量标准和加强监督农业安全生产提供依据。 方法 2012—2016年采集杭州市富阳区农贸市场和生产基地等销售的新鲜蔬菜共671份,按照NY/T 761-2008 《蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留的测定》方法对30种常用农药的残留量进行检测,并以GB 2763-2014 《食品安全国家标准 食品中农药最大残留限量》作为判定标准。 结果 对671份蔬菜样品进行农药检测和数据分析显示,检出农药阳性样品146份,检出率为21.8%,超限量样品为15份,占2.2%。共检测出农药种类20种,频次182。其中,叶菜类蔬菜中农药检出率最高,达30.3%;瓜类蔬菜中农药检出率仅为4.0%。 结论 部分蔬菜中农药残留较高,甚至超出国家标准,农业安全生产监督仍需加强。国家标准中缺乏部分农药在特定蔬菜中的限量标准要求,急需完善。     

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%).     

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%).     

成都市售果蔬中农药残留水平分析及慢性膳食风险评估

了解成都市果蔬中农药残留污染现状及其对成都市居民的膳食风险水平。采集成都市果蔬大型农贸市场和超市的9类果蔬共203份样品,采用改良的GB 23200.113-2018 QuEChERS前处理方法,结合气相色谱-三重四级杆串联质谱对48种农药进行检测,分析成都市果蔬中农药残留现状,并结合大城市居民的果蔬消费情况和食品安全指数法对成都市居民从果蔬中摄入农药风险进行慢性膳食暴露评估。结果显示:48种农药在0.025~25 μg/kg范围内线性关系良好,相关系数均大于0.99,回收率为60.1%~117.7%,相对标准偏差均小于10%,方法定量限为0.083~3.3 μg/kg,可以满足果蔬中农药痕量检测的要求。203份果蔬样品中农药残留检出率为50.2%,共检出6种农药,均未超标,其中吡唑醚菌酯检出率最高,为29.1%。不同种类果蔬受农药污染程度不同,以草莓为代表的浆果和其他小型类水果检出率最高,达91.7%。慢性膳食暴露评估结果显示所有检出农药的食品安全指数值为0.00002~0.004,均小于1,但炔螨特的日摄入量最高,为0.00257 mg/d,应重点关注。     

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。     

唐山地区韭菜农药残留检测分析及膳食摄入风险评估

为了解唐山地区流通韭菜的农药残留状况与民众的膳食摄入风险,该研究采用高效液相色谱-串联质谱仪(HPLC-MS/MS)和气相色谱仪(GC)对2020年在唐山地区采集的415个韭菜样品分别进行了68种农药残留定性定量检测,并对韭菜样品中检出的农药进行风险评估.结果 表明,415个韭菜样品共计检出41种农药残留,检出率为69...     

Pesticide residues in oranges from Valencia (Spain)

One hundred and fifty citrus samples from an agricultural co-operative of the Valencian Community (Spain) were analysed for pre- and post-harvest pesticide residues using high performance liquid chromatography and gas chromatography. Among the residues from post-harvest treatments, imazalil was detected in 112 (74.7%) samples at a mean level of 1.2mg/kg, thiabendazole in 21 (14.0%) samples at a mean level of 0.47mg/kg and carbendazim in 5 (3.3%) samples at a mean level of 1.05mg/kg. Among the residues from preharvest treatment, dicofol was detected in 28 (18.7%) samples at a mean level of 0.28mg/kg, chlorpyriphos in 19 (12.7%) samples at a mean level of 0.16mg/kg and endosulfan in 11 (7.3%) at a mean level of 0.27mg/kg. Most of the samples contained residues of various pesticides and six samples (4.0%) exceeded the European Union Maximum Residue Limit (MRL). The pesticides that surpassed the MRLs were chlorpyriphos in five samples and dicofol in one.     

Validation of a headspace solid-phase microextraction procedure with gas chromatography-electron capture detection of pesticide residues in fruits and vegetables

Headspace solid-phase microextraction (HS-SPME) was evaluated for the determination of pesticide residues in fruits and vegetables by gas chromatography with an electron capture detector (GC-ECD). The fibre used was coated with polydimethylsiloxane (100 μm thickness) and the analytical conditions employed have been developed and optimised in a previous work [Chai, M. K., Tan, G. H., & Asha, L. (2008). Optimisation of headspace solid-phase microextraction for the determination of pesticide residues in vegetables and fruits. Analytical Sciences, 24 (2), 273–276]. The results show that the HS-SPME procedure gave a better linear range, accuracy, precision, detection and quantification limits and is adequate for analysing pesticide residues in fruits and vegetables. The average recoveries obtained for each pesticide ranged between 71% and 98% at three fortification levels with the relative standard deviation of less than 5%. Repeatability (0.3–3.7%) and intermediate precision (0.8–2.5%) were shown to be satisfactory. The limits of detection (0.01–1 μg L⁻¹) and the limits of quantification (0.05–5 μg L⁻¹) of these pesticides were much lower than the maximum residue levels (MRL), allowed for fruits and vegetables in Malaysia.     

QuEChERS-气相色谱-三重四极杆-串联质谱法测定果蔬中222种农药残留

目的 建立一种QuEChERS前处理结合气相色谱-三重四极杆串联质谱(gas chromatography-triple quadrupole tandem mass spectrometry, GC-MS/MS)快速测定水果、蔬菜中222种农药残留的分析方法。方法 样品用乙腈均质提取, QuEChERS技术提取和净化, 经气相色谱分离, 用GC-MS/MS在动态多反应离子监测(dynamic multiple reaction monitoring, dMRM)下进行检测, 基质匹配标准溶液进行内标法测定。结果 222种农药在0.005~0.2 mg/L的浓度范围内线性关系良好, 相关系数(r2)均≥0.990, 不同基质在0.01、0.05、0.1 mg/kg的添加水平下大部分农药的平均回收率为90%~120%, 相对标准偏差(relative standard deviation, RSD)为1.2%~8.9%, 方法的定量限(limit of quantitation, LOQ)为0.01~0.02 mg/kg。结论 该法快速、准确、灵敏、重现性较好、适用于大批量水果、蔬菜中农药残留的快速筛查分析。