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1.
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%).  相似文献   

2.
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.  相似文献   

3.
Drinking water, cowpea and maize grains were sampled in some potentially exposed agro-ecological areas in Togo and analysed for their contamination by some common organochlorine pesticides. A total of 19 organochlorine pesticides were investigated in ten subsamples of maize, ten subsamples of cowpea and nine subsamples of drinking water. Analytical methods included solvent extraction of the pesticide residues and their subsequent quantification using gas chromatography-mass spectrometry (GC/MS). Estimated daily intakes (EDIs) of pesticides were also determined. Pesticides residues in drinking water (0.04–0.40 µg l?1) were higher than the maximum residue limit (MRL) (0.03 µg l?1) set by the World Health Organization (WHO). Dieldrin, endrin, heptachlor epoxide and endosulfan levels (13.16–98.79 µg kg?1) in cowpea grains exceeded MRLs applied in France (10–50 µg kg?1). Contaminants’ levels in maize grains (0.53–65.70 µg kg?1) were below the MRLs (20–100 µg kg?1) set by the Food and Agriculture Organization (FAO) and the WHO. EDIs of the tested pesticides ranged from 0.02% to 162.07% of the acceptable daily intakes (ADIs). Population exposure levels of dieldrin and heptachlor epoxide were higher than the FAO/WHO standards. A comprehensive national monitoring programme on organochlorine pesticides should be undertaken to include such other relevant sources like meat, fish, eggs and milk.  相似文献   

4.
The applicability of liquid chromatography coupled to hybrid quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) for the quantitative analysis of pesticide residues in vegetables and fruits was demonstrated. The LC-QTOF-MS parameters, such as cone voltage, capillary voltage, collision energy and mass extraction window, were carefully optimised for the analysis of pesticide residues. The LC-QTOF-MS method was validated for 149 pesticides in four vegetables and fruits, i.e. apple, potato, cabbage and spinach, at a spiking level of 0.01 mg kg?1. The samples were prepared according to the Japanese official multi-residue method with a modification to the column clean-up procedure. Of the 149 pesticides, recoveries in the range of 70–120% were achieved for 147 pesticides in apple, 145 in potato, 141 in cabbage and 131 in spinach, with intra-day precisions (RSDs) of < 25% and inter-day precisions (RSDs) of < 30%, which are within the acceptable range given in the Japanese method validation guideline. Matrix effects were negligible for the majority of the target pesticides. Except for spiroxamine in spinach, no interfering peaks were observed in the blank samples. The target pesticides, except those with low sensitivity, achieved calibration curves with satisfactory linearity, with correlation coefficients (r) greater than 0.995 in the concentration range of 0.002–0.1 μg ml?1. Furthermore, the majority of the target pesticides provided more than one fragment ion or isotope ion that could be used for confirmation. The overall results suggest that LC-QTOF-MS is a powerful tool for the quantification of pesticide residues in vegetables and fruits at the level of 0.01 mg kg?1.  相似文献   

5.
This paper describes a comparison of adaptations of the QuEChERS (quick, easy, cheap, effective, rugged and safe) approach for the determination of 14 organochlorine pesticide (OCP) residues in strawberry jam by concurrent use of gas chromatography (GC) coupled to electron capture detector (ECD) and GC tandem mass spectrometry (GC-MS/MS). Three versions were tested based on the original QuEChERS method. The results were good (overall average of 89% recoveries with 15% RSD) using the ultrasonic bath at five spiked levels. Performance characteristics, such as accuracy, precision, linear range, limits of detection (LOD) and quantification (LOQ), were determined for each pesticide. LOD ranged from 0.8 to 8.9?µg?kg?1; LOQ was in the range of 2.5–29.8?µg?kg?1; and calibration curves were linear (r 2?>?0.9970) in the whole range of the explored concentrations (5–100?µg?kg?1). The LODs of these pesticides were much lower than the maximum residue levels (MRLs) allowed in Europe for strawberries. The method was successfully applied to the quantification of OCP in commercially available jams. The OCPs were detected lower than the LOD.  相似文献   

6.
A multi-residue method using selected ion monitoring mode GC/MS has been developed for the quantitative analysis of residue levels of 23 widely used pesticides in fresh peaches produced under integrated crop management process (ICM). The proposed methodology involved a sample extraction procedure using liquid–liquid partition with acetonitrile followed by a clean-up step based on solid-phase extraction (SPE). Fortification studies were performed at different concentration levels for various types of peaches that differ in properties, such as appearance, flavor and pit. The data showed that the different peach matrices had no significant effect on recoveries. Recoveries were greater than 80% for most of the pesticides with a RSD below 18%. The limits of quantification (LOQs) were in the range 0.002–0.050 mg kg?1, depending on the compound. To assess method performance with real samples and determine whether pesticide concentrations in peaches exceed their maximum residue levels (MRLs), the proposed method was successfully applied to the analysis of 104 fruit samples collected under integrated pest management (IPM) production during the 2006 cultivation period. Residues detected were lower than those established by legislation for all pesticides, except diazinon, where one positive sample was detected at a level of 0.03 mg kg?1.  相似文献   

7.
A rapid, high-throughput method employing ultra-performance liquid chromatography with tandem quadrupole mass spectrometry (UPLC-MS/MS) was developed and optimized for simultaneous quantification and confirmation of 64 pesticide residues and their toxic metabolites in fruit extracts prepared by a buffered QuEChERS procedure. The total time required for UPLC-MS/MS analysis was 8 min plus 2 min for re-equilibration to the initial UPLC conditions. Performance characteristics were determined for apple extracts spiked at 10 µg kg?1. The repeatability of measurements expressed as relative standard deviations was in the range 1.5–13% at this level for most analytes. Thanks to very low limits of quantification (<10 µg kg?1for the majority of pesticides), an optimized method allows for the reliable control of not only common maximum residue limits (MRLs) set by European Union regulation for various pesticides/fruit combinations, but also of a uniform MRL of 10 µg kg?1endorsed for baby food.  相似文献   

8.
More than 90% of the pesticides residues in apples are located in the peel. We developed a gas chromatography/ion trap tandem mass spectrometry method for investigating all detectable residues in the peel of 3 apple varieties. Sample preparation is based on the use of the Quick Easy Cheap Effective Rugged and Safe method on the whole fruit, the flesh, and the peel. Pesticide residues were quantified with solvent‐matched and matrix‐matched standards, by spiking apple sample extracts. Matrix effects dependent on the type of extract (fruit, flesh, or peel) and the apple variety were detected. The best data processing methods involved normalizing matrix effect rates by matrix‐matched internal/external calibration. Boscalid, captan, chlorpyrifos, fludioxonil, and pyraclostrobin were the most frequently detected pesticides. However, their concentrations in the whole fruit were below European maximum residue levels. Despite negative matrix effects, the residues in peel were detected at concentrations up to 10 times higher than those in whole fruits. Consequently, other pesticide residues present at concentrations below the limit of quantification in the whole fruit were detected in the peel.  相似文献   

9.
This work investigates the content of feruloylquinic (FQA), caffeoylquinic (CQA) and dicaffeoylquinic (diCQA) acids in the peel, pulp and seed of 22 tropical fruits from Brazil. 3‐CQA, 4,5‐diCQA and 4‐ and 5‐FQA were not detected in any of the fruits analysed. Relatively small amounts of 4‐CQA (4.0–48.7 mg kg?1) were found in the peel and/or pulp of seven of the fruits; only the peel of Artocarpus heterophyllus was significantly (p < 0.05) richer in this acid (1000 mg kg?1). The distribution of 3,4‐ and 3,5‐diCQA in different parts of the fruits was relatively poor, only reaching levels of up to 16.4 mg kg?1. The peel of A heterophyllus also showed the highest amount of 5‐CQA (13 000 mg kg?1), while the seed of most fruits generally contained a lower amount of this acid than the peel or pulp. On the basis of the 5‐CQA content found in the pulp, 15 of the fruits were classified as follows: very low concentration (4.4–15.8 mg kg?1), low concentration (28.9–66.4 mg kg?1), medium concentration (132 mg kg?1), high concentration (473–474 mg kg?1) or very high concentration (1730 mg kg?1); however, no 5‐CQA was detected in the pulp of the other seven fruits. Thus 5‐CQA was the major chlorogenic acid present in most of the tropical fruits studied and was generally accompanied by small amounts of 4‐CQA and 3,4‐ and 3,5‐diCQA. © 2002 Society of Chemical Industry  相似文献   

10.
A QuEChERS procedure for the simultaneous determination of pyrimethanil, cyprodinil, mepanipyrim and its metabolite (M31) in fresh and processed fruit and vegetables was developed using ultra-performance liquid chromatography/tandem mass spectrometry (UPLC-MS/MS). The determination of the four target compounds was achieved in less than 6.0 min using an electrospray ionisation source in positive mode. The limits of detection (LODs) were below 0.4 μg?kg?1, while the limits of quantification (LOQs) did not exceed 1.5 μg?kg?1 for all studied matrices. Good linearity of the calibration curves was obtained over the range from 0.002 to 2 mg?kg?1, with correlation coefficients higher than 0.999. The average recoveries of this method in apple, peach, cabbage and tomato at the five spiked levels (0.002, 0.01, 0.05, 0.20 and 2.0 mg?kg?1) ranged from 81.5% to 107.3% with relative standard deviations (RSDs) in the range of 1.5–13.9% (n = 5) for all analytes. Residue levels of anilinopyrimidine fungicides in fresh and home-processed apple, peach, cabbage and tomato were also studied. The results indicate that residue levels are significantly reduced following washing, peeling and boiling, and there is no toxic metabolite of mepanipyrim (M31) which is detected during boiling. This study provides a theoretical basis for China to draw up maximum residue limits (MRLs) and protect consumers from the negative health effects of pesticide residues detected in fruit and vegetables.  相似文献   

11.
目的评估目前山东主要苹果产区的农药残留水平,为农药残留监管提供科学依据。方法对采自山东苹果主产区的110个苹果样品运用现有的标准方法进行102种农药残留分析检测,利用急性参考剂量(acute reference dose,ARf D)和国家估计短期摄入量(international estimated short-term intake,IESTI)公式评估苹果农药累积急性风险。结果山东省苹果共检出26种农药残留,多残留(2种农残及以上)样品占样品总数的78%,所有样品检出农药残留量均未超过规定的最大残留限量值;检出苹果上禁用农药灭多威和未登记农药噻嗪酮、螺螨酯、杀铃脲;有机磷类、菊酯类、三唑类和烟碱类农药在山东苹果中累积急性膳食摄入风险(%ARf D值)分别为37.7%、7.37%、0.28%和1.53%。结论山东省苹果农药残留种类较多,残留水平不高,有机磷类、菊酯类、三唑类和烟碱类农药累计急性摄入风险较小,但需重点关注苹果上禁用农药和未登记农药。  相似文献   

12.
Several tropical fruits have been described as natural sources of dietary fibre (DF) and phenolic compounds, associated with different health effects. The aim of this work was to ascertain the DF, phenolic compounds content (including non‐extractable polyphenols, mostly associated with DF) and antioxidant capacity in acerola fruits and cashew apples from selected clones. ‘BRS 236’ acerola fruits presented a high antioxidant capacity because of the combination of both extractable polyphenols and l ‐ascorbic acid (providing together a Folin value of 170 kg?1 g d.m.). ‘CCP 76’ cashew apples contained 28 g kg?1 d.m. of extractable polyphenols and 13 g kg?1 d.m. of ascorbic acid as well as a high amount of non‐extractable condensed tannins (52 g kg?1 d.m.). DF content was of 260 g kg?1 d.m. in acerola fruit and of 209 g kg?1 d.m. in cashew apple. Acerola fruits and cashew apple should therefore be considered as new natural sources of DF and phenolic compounds.  相似文献   

13.
The goal of this research was to evaluate the application of Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method for the determination of organochlorine, organophosphate, and carbamate pesticides in fatty animal matrices such as liver of chicken obtained from National Research Institute of Animal Production in Balice (Poland). Pesticides extraction effectiveness was evaluated at two different spiking levels (0.010 and 0.020 mg kg?1) and efficiency of the dispersive solid-phase extraction (d-SPE) clean-up step was evaluated by comparison adding different d-SPE sorbent combinations (PSA?+?GCB, PSA?+?C18, PSA?+?SAX, and PSA?+?NH2). The analysis of pesticide residues was performed by gas chromatography ion trap mass spectrometry (GC/IT-MS). The linear relation was observed from 0 to 400 ng mL?1 and the determination coefficient R 2?>?0.997 in all instances for all target analytes. Better recoveries were obtained in samples at 0.020 mg kg?1 spiking level. The recoveries were in the range 70–120 %, with relative standard deviation (RSD) values lower than 15 % at 0.020 mg kg?1 spiking level for most pesticides. Similar recovery ratios were obtained with the four different combinations of sorbents tested in the clean-up step, with better precision when the (PSA?+?SAX) combination was tested. Limits of detection (LODs) ranged from 0.001 to 0.005 mg kg?1 and limits of quantification (LOQs) ranged from 0.003 to 0.015 mg kg?1. The proposed method was successfully applied analyzing pesticide residues in real chicken liver samples; detectable pesticide residues were observed, but in all of the cases, the contamination level was lower than the default maximum residue levels (MRLs) set by European Union (EU), Regulation (EC) N 396/2005.  相似文献   

14.
A study was conducted to analyse market-regulated heavy metals (lead, mercury and cadmium), organochlorine pesticides and total polychlorinated biphenyls (PCBs) in samples of 38 farmed fish comprising Nile tilapia (Oreochromis niloticus) (20 samples) and African catfish (Clarias gariepinus) (18 samples) from ten selected fish farms in Uganda. The goal of this case study was to understand the safety of aquaculture products from Sub-Saharan Africa. Lead was detected in all the 38 samples (maximum = 1.08 mg kg?1 (dry weight)), mercury in 31 out of 38 samples (maximum = 0.35 mg kg?1 (dry weight)), and cadmium in two samples (maximum = 0.03 mg kg?1 (dry weight)). Total levels of PCBs were below the limit of detection of 0.02 mg kg?1 (wet weight) in all the samples. Traces of 4,4′-dichloro-diphenyldichloroethylene (DDE) were detected in ten out of 38 samples (maximum = 0.01 mg kg?1 (wet weight)) making it the most prevalent organochlorine pesticide. Other pesticides detected were: 4,4′-dichloro-diphenyl-trichloroethane (DDT) and endosulfan sulphate, which were found in one fish sample (both 0.002 mg kg?1 (wet weight)). There was no statistically significant difference between the levels of lead and mercury in catfish and tilapia (t-test at p = 0.05). More catfish samples (eight) contained DDE as compared with tilapia (two). Cadmium, DDT and endosufan sulphate were only detected in catfish implying that catfish is more prone to contamination than tilapia. The levels of contaminants were below the US Food and Drug Administration (USFDA) action levels and European Union maximum residue limits (MRLs), indicating that such fish have the potential for export to these markets.  相似文献   

15.
The phenolics in 20 apple cultivars comprising 19 English cider apple varieties and one dessert apple variety were analysed by high‐performance liquid chromatography/tandem mass spectrometry. The cider varieties contained higher levels than the dessert apple and the peel was richer in phenolics than the flesh. The phenolic concentrations ranged between 230 and 4920 mg kg?1 fresh weight in the flesh and between 546 and 6306 mg kg?1 fresh weight in the peel. Fifteen compounds from five different phenolic groups, flavan‐3‐ols, flavonols, anthocyanins, hydroxycinnamates and dihydrochalcones, were detected. The major components in the flesh were 5‐O‐caffeoylquinic acid, procyanidin B2 and (?)‐epicatechin, while (?)‐epicatechin and quercetin glycosides predominated in the peel. Copyright © 2007 Society of Chemical Industry  相似文献   

16.
In northern Cameroon, the misuse of pesticides for pest control is common among small-scale farmers. Therefore, monitoring of pesticide residues was carried out on stored maize, cowpea and millet from eight localities. The determination of residues of organochlorines (lindane, α-endosulfan and β-endosulfan), organophosphorus compounds (malathion and pirimiphos-methyl), synthetic pyrethroids (permethrin) and carbamates (carbufuran) was performed using GC–ECD/NPD and GC–MS for confirmation. Organochlorine pesticides were detected more frequently and in higher concentrations, ranging from 0.02 ± 0.01 mg kg?1 for β-endosulfan in millet to 9.53 ± 4.00 mg kg?1 lindane in maize, than organophosphorus compounds, with concentrations varying from 0.04 ± 0.03 mg kg?1 for pirimiphos methyl to 0.23 ± 0.38 mg kg?1 for malathion in maize. Permethrin was found only in maize at 0.39 ± 0.23 mg kg?1. No carbofuran was found. More than 75% of samples contained pesticide residues above the maximum residue limit (MRL); showing a potential human dietary risk related to consumption of these grains.  相似文献   

17.
Between 1978 and 1986, 305 samples of apples were monitored for the residues of a wide range of pesticides used in their production. Three (1%) contained residues above the maximum residue limits (MRL) permitted under the Canadian Food and Drug Act and regulations; two involved phosalone at 5.9 and 6.2 mg/kg respectively and one involved diphenylamine at 6.7 mg/kg when the MRL was 5.0 mg/kg for both compounds. Low residues of dicofol, endosulfan, phosalone, phosmet, captan, daminozide and diphenylamine were frequently found; however they were well below the MRLs. These residue levels were correlated with survey data on the areas of the apple crop treated with specific pesticides. Residues of carbaryl, diazinon, ethion, azinophosmethyl, parathion, and dithiocarbamate fungicides were found occasionally; all were well below the MRLs and correlated with the pattern of use. No residues of PCB were found to a limit of detection of 0.01 mg/kg.  相似文献   

18.
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%).  相似文献   

19.
The fast measurement of pesticide residues on fruits peels is crucial, for it is harmful for both human health and environment. In this study, we used apples and chlorpyrifos as the research materials and analyzed the volatiles from apples via its infrared spectra. As the low concentration of the volatiles, multi-reflecting mirrors were used to enhance the sensitivity of the spectroscopy system. From the experiment, two obvious spectral characteristics from chlorpyrifos, 990–2830 and 1259–1227 cm?1, has been observed. By analyzing the infrared spectra of the volatiles released from chlorpyrifos with different dilution ratios on the apple peels, we found the spectral intensities increased with the chlorpyrifos concentrations. The results were further analyzed using chemometrics, it is demonstrated that there are obvious spectral differences among the apples sprayed with 1:20, 1:100, and 1:1000 chlorpyrifos and clean apples. The above four groups of the samples can be classified using principal component analysis (PCA). This study demonstrated that gas-phase long-path infrared spectroscopy is an effective method to detect the pesticide residues on fruits peels, with the advantages of no sample treatment and fast. To the best of our knowledge, this is the first study to detect pesticide residues on fresh and untreated apples using infrared spectroscopy via its volatiles.  相似文献   

20.
During 3 years of a monitoring programme, 522 samples of fresh apples, six brands of fruit purées and various types of fruit baby food prepared from these materials were analysed. Each sample was examined for the presence of 86 GC amenable pesticide residues. The reporting limits of the procedure employed for sample analyses were in the range 0.003-0.01 mg kg(-1). Pesticide residues were detected in 59.5% of the samples of fresh apples. However, maximum residue levels (European Union MRLs) were exceeded only in 1.4% of samples. The levels of residues in 'positive' fruit purées were substantially lower, overall with residues detected in 33% of samples. Fruit baby food represented the commodity with the lowest incidence of residues being detected in only 16% of samples. The 0.01 mg kg(-1) MRL was exceeded in 9% of these products. Multiple residues were found in 25% of fresh apples and in 10% of fruit purées. None of fruit baby food samples contained more than a single residue. Organophosphorus insecticides and fungicides representing phtalimides, sulphamides and dicarboximides were the most frequently found residues. To obtain more knowledge on the fate of residues during fruit baby food production, processing experiments employing apples with incurred residues (fenitrothion, phosalone and tolylfluanid) were conducted. Washing of apples did not significantly reduce the content of pesticides. Steam boiling followed by removal of peels/stems was identified as the most efficient steps in terms of residues decrease (phosalone) or complete elimination (fenitrothion and tolylfluanid).  相似文献   

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