Food and Drug Administration pesticide residue monitoring of foods: 1983-1986

Pesticide residues in foods are reported for the 4-year period 1982-1986 [fiscal years (FY) 83-86]. Results were summarized from the 2 complementary approaches that make up the Food and Drug Administration's (FDA) pesticide residue monitoring program. Under regulatory monitoring, which focuses on residues in raw agricultural commodities, a total of 49,055 samples (27,700 domestic and 21,355 import) that included fresh fruits and vegetables, grains and grain products, milk and dairy products, seafoods, and a variety of processed foods were analyzed. No residues were found in 60 and 48% of the domestic and import samples, respectively, compared with 55 and 44% in FY78-82. About 3% of the domestic and 5% of the import samples were violative. In FY78-82, about 3 and 7% were violative, respectively. The other FDA monitoring approach, the Total Diet Study, was revised in April 1982 to expand coverage of age/sex groups, use updated diets, and provide for analysis of individual foods. Results from monitoring under this modified approach and from regulatory monitoring continued to demonstrate that pesticide residues in the U.S. food supply were well below regulatory limits, and dietary intakes were many times lower than the Acceptable Daily Intakes established by international agencies.     

FDA monitoring program. Residues in foods--1990.

In 1990, under regulatory monitoring, a total of 19,962 samples of domestically produced food from all 50 states and Puerto Rico and imported food from 92 countries were analyzed by FDA for pesticide residues. Of these, 19,146 were surveillance samples, which are collected when there is no suspicion of a pesticide problem. No residues were found in 60% of domestic surveillance samples and in 64% of import surveillance samples. Of the 19,146 surveillance samples, 2.8% were violative. Under the incidence/level aspect of monitoring, 172 samples of fish/shell-fish, 330 samples of whole milk, and 3502 samples of processed foods including baby foods were analyzed for pesticide residues. Findings from these projects were consistent with regulatory monitoring data. The findings of the 1990 Total Diet Study are evidence that actual dietary intakes of pesticides are generally well below the standards established by FAO/WHO and by EPA. The 1990 results are similar to those obtained in earlier years and demonstrate the continuing safety of the food supply relative to pesticide residues.     

State findings on pesticide residues in food--1988 and 1989

Findings of pesticide and related chemical residues are presented for 27,065 samples of foods collected and analyzed in 10 state food laboratories over 1988 and 1989 (fiscal years (FY) 88 and 89). These laboratories conduct food regulatory programs compatible with national programs of the U.S. Food and Drug Administration. Of the findings, 6325 samples contained detectable levels of 1 or more pesticide analytes and 418 (or 1.5%) of the total number of samples were deemed to be of regulatory significance.     

The FDA pesticides program: goals and new approaches

The U.S. Food and Drug Administration (FDA) has carried out a large-scale monitoring program for pesticide residues in foods since the 1960s. The program has evolved continuously as evidenced by a number of recently incorporated modifications and initiatives. Included are greater emphasis on imports; increased and more specific targeting of pesticide/commodity combinations by geographic area or country; development of individual district sampling plans for domestic and imported foods; expanded use of single residue methods; linkage of information on foreign pesticide usage with food import volumes; development of an analytical methods research plan; and increased cooperative sampling and data exchange with the states. Initiatives to acquire and utilize private sector and other monitoring data are being explored, and aggressive steps are being taken to inform the public of FDA monitoring results in a timely and understandable manner.     

农药残留风险评估在蔬菜水果和食用菌监测中的应用研究

为了解我国西北地区蔬菜水果和食用菌的质量安全情况及暴露风险,本试验从2018至2020年在我国甘肃省平凉市进行样品抽取,共测定2 435份蔬菜水果和食用菌样品中46种农药残留的含量.通过农药残留风险评估方法分析了 9类别蔬菜水果和食用菌中农药残留的分布和相关性,并对蔬菜和水果中农药残留情况进行了风险排序,以及暴露风险、...     

Pesticide residues in imported, organic, and "suspect" fruits and vegetables

Consumers are frequently urged to avoid imported foods as well as specific fruits and vegetables due to health concerns from pesticide residues and are often encouraged to choose organic fruits and vegetables rather than conventional forms. Studies have demonstrated that while organic fruits and vegetables have lower levels of pesticide residues than do conventional fruits and vegetables, pesticide residues are still frequently detected on organic fruits and vegetables; typical dietary consumer exposure to pesticide residues from conventional fruits and vegetables does not appear to be of health significance. Similarly, research does not demonstrate that imported fruits and vegetables pose greater risks from pesticide residues than do domestic fruits and vegetables or that specific fruits and vegetables singled out as being the most highly contaminated by pesticides should be avoided in their conventional forms.     

Levels of pesticide residues in Egyptian human milk samples and infant dietary intake

Contamination of human milk with residues of organochlorine pesticides and polychlorinated biphenyls was studied in a series of investigations concerned with the monitoring of these chemicals in Egyptian food. The DDT complex was the most frequently found pesticide, followed by total hexachlorocyclohexane isomers. Heptachlor and its epoxide, dieldrin, hexachlorobenzene, and oxychlordane were also found but less frequently. Estimated dietary intakes (EDIs) of these contaminants by the breast-fed infants were compared to acceptable daily intakes (ADIs). EDIs of DDT complex, lindane (gamma-HCH), heptachlor + heptachlor epoxide, and oxychlordane were below ADIs. Dieldrin EDI exceeded the acceptable daily intake.     

Immunoassay of pesticides

Determination of the presence and levels of pesticide residues in food is fundamental in monitoring and regulatory programs. Residues are separated from the food matrix by solvent extraction, followed by cleanup steps. The residues are most often identified and quantitated by instrumental analysis, usually liquid or gas chromatography. Extraction and cleanup are often laborious and time-consuming; determination requires expensive, sophisticated instrumentation. There is a need for rapid, easily performed tests, such as immunoassays, that could be used for screening under field conditions or for quantitation of residues in foods in the laboratory. Although a large number of immunoassays have been developed for pesticide chemicals, very few have been specifically applied to foods, and only a very small number are currently available commercially. The agencies charged with monitoring and regulatory responsibilities--Environmental Protection Agency, Food and Drug Administration, and U.S. Department of Agriculture--as well as professional societies such as AOAC and the International Union of Pure and Applied Chemistry, are investigating and developing guidelines for test kit evaluation and standards to be met before a kit can be accepted as a practical and useful method of analysis for use in their programs.     

Pesticide residue findings by the Luke method in domestic and imported foods and animal feeds for fiscal years 1982-1986

Nearly 20,000 samples of food and feed commodities were analyzed for pesticide residues by the U.S. Food and Drug Administration Los Angeles District Laboratory during the 5-year study period 1981-1986. The resultant data base has been summarized to provide separate residue information for domestic and imported samples. The overall violation rates for domestic and imported samples collected on a surveillance basis were 3.0 and 2.6%, respectively. For domestic and imported samples collected on a compliance basis, the overall violation rates were 19.7 and 17.5%, respectively.     

Evaluation of capillary gas chromatography for pesticide and industrial chemical residue analysis. II. Comparison of quantitative results obtained on capillary and packed columns

Results of pesticide and industrial chemical residue determinations, using both capillary and packed column gas chromatography (GC), in 3 Food and Drug Administration (FDA) laboratories have been compiled and compared. Samples consisted of food products collected for routine residue screening by the respective laboratories. Extracts were prepared by conventional multiresidue methodology. Capillary column systems and operating conditions were selected at the discretion of each laboratory and were therefore variable, although split/splitless injectors in the split mode were used with prescribed precautions in all cases. Packed column systems were operated as specified in the FDA Pesticide Analytical Manual (PAM). Overall correlation between the 2 systems, expressed as the average ratio of packed column result to capillary column result, was 0.99 for 120 determinations in 41 samples. The higher resolving power of the capillary systems allowed quantitation of several residues that were incompletely separated and therefore unquantifiable using the packed columns. Capillary column GC with the split injection technique, used with appropriate precautions, was found to be both reliable and advantageous for regulatory determination of pesticide and industrial chemical residues in foods and feeds.     

Improving the nutritional status of food-insecure women: first, let them eat what they like

OBJECTIVE: To determine the extent to which identified nutrient inadequacies in the dietary intakes of a sample of food-insecure women could be ameliorated by increasing their access to the 'healthy' foods they typically eat. DESIGN: Merged datasets of 226 food-insecure women who provided at least three 24-hour dietary intake recalls over the course of a month. Dietary modelling, with energy adjustment for severe food insecurity, explored the effect of adding a serving of the woman's own, and the group's typically chosen, nutrient-rich foods on the estimated prevalence of nutrient inadequacy. SETTING AND SUBJECTS: One study included participants residing in 22 diverse community clusters from the Atlantic Provinces of Canada, and the second study included food bank attendees in Toronto, Ontario, Canada. Of the 226 participants, 78% lived alone with their children. RESULTS: While nutritional vulnerability remained after modelling, adding a single serving of either typically chosen 'healthy' foods from women's own diets or healthy food choices normative to the population reduced the prevalence of inadequacy by at least half for most nutrients. Correction for energy deficits resulting from severe food insecurity contributed a mean additional 20% improvement in nutrient intakes. CONCLUSIONS: Food-insecure women would sustain substantive nutritional gains if they had greater access to their personal healthy food preferences and if the dietary compromises associated with severe food insecurity were abated. Increased resources to access such choices should be a priority.     

Variations in isoflavone levels in soy foods and soy protein isolates and issues related to isoflavone databases and food labeling

The reliability of databases on the isoflavone composition of foods designed to estimate dietary intakes is contingent on the assumption that soy foods are consistent in their isoflavone content. To validate this, total and individual isoflavone compositions were determined by HPLC for two different soy protein isolates used in the commercial manufacture of soy foods over a 3-year period (n = 30/isolate) and 85 samples of 40 different brands of soy milks. Total isoflavone concentrations differed markedly between the soy protein isolates, varying by 200-300% over 3 years, whereas the protein content varied by only 3%. Total isoflavone content varied by up to 5-fold among different commercial soy milks and was not consistent between repeat purchases. Whole soybean milks had significantly higher isoflavone levels than those made from soy protein isolates (mean +/- SD, 63.6 +/- 21.9 mg/L, n = 43, vs 30.2 +/- 5.8 mg/L, n = 38, respectively, p < 0.0001), although some isolated soy protein-based milks were similar in content to "whole bean" varieties. The ratio of genistein to daidzein isoflavone forms was higher in isolated soy protein-based versus "whole bean" soy milks (2.72 +/- 0.24 vs 1.62 +/- 0.47, respectively, p < 0.0001), and the greatest variability in isoflavone content was observed among brands of whole bean soy milks. These studies illustrate large variability in the isoflavone content of isolated soy proteins used in food manufacture and in commercial soy milks and reinforce the need to accurately determine the isoflavone content of foods used in dietary intervention studies while exposing the limitations of food databases for estimating daily isoflavone intakes.     

低糖姜脯加工过程对甲基硫菌灵和多菌灵残留的影响

为研究低糖姜脯加工过程对生姜中甲基硫菌灵和多菌灵残留量的影响,以江永香姜为原料,通过浸药方式强化初始残留量,采用液相色谱串联质谱法测定各主要加工工序中2种农药残留量的变化,并计算2种农药在各工序中的加工因子。结果表明,在低糖姜脯加工过程中,除2次干燥工序,其他加工工序对甲基硫菌灵和多菌灵的残留水平均有一定的降低作用,全果清洗步骤多菌灵的去除率为31.1%,甲基硫菌灵的去除率高达62.3%;去皮工序甲基硫菌灵和多菌灵的去除率分别为82.0%和72.9%,漂烫工序甲基硫菌灵和多菌灵的去除率分别为36.8%和77.3%,硬化、超声辅助加热渗糖和上胶衣过程均对甲基硫菌灵和多菌灵的去除有一定的积极影响。在整个加工过程中,各工序姜脯样品的加工因子均小于1,低糖姜脯成品中的甲基硫菌灵和多菌灵的加工因子分别为0.010和0.023,表明整个加工过程可以显著降低姜脯中甲基硫菌灵和多菌灵的残留量(P<0.05)。本研究结果为生姜加工工艺的优化和农药残留的膳食暴露风险评估提供了数据支撑和参考。     

Comparison of accelerator mass spectrometry with gas chromatography for the determination of pesticide residues in individual items in the diets of wild birds and mammals

Methods to refine the assessment of exposure of wild birds and mammals to pesticides required measurement of pesticide residues in very small samples of their diets. Sample sizes were in the 1-100 mg range, and the target residue for measurement was 0.01 mg/kg. Gas chromatography-mass spectrometry (GC-MS) with large volume injection was compared with the use of an accelerator mass spectrometer (AMS) to measure residues of pesticide labeled at near-background levels with carbon-14. The GC-MS method was able to detect residues down to 0.1 ng per item of diet, and the AMS detected the radiolabel down to 1 mBq (0.06 disintegration per minute, 1 ng of pesticide at the specific activity used) per sample. The target residue level was achieved by the GC-MS method for samples down to 10 mg. The GC method appeared to be best suited to monitoring residues in field studies, and the AMS shows great potential for use in laboratory experiments concerning pesticide degradation.     

Urea enzymatic dialysis procedure for determination of total dietary fiber

A method that uses urea and enzymes for determination of total dietary fiber (TDF) in foods has been developed and compared with the AOAC enzymatic-gravimetric method (43.A14-43.A20). In the evaluation, results for crude protein and ash contamination were higher by the AOAC method, particularly for samples that form gels during ethanol precipitation. The new urea enzymatic dialysis (UED) method quantitatively recovered, with less variation, more of the purified and semipurified dietary fiber products. TDF recoveries for carboxymethylcellulose and locust bean gum were 98% (SD 3.3) and 95% (SD 6.1) by the AOAC method and 99% (SD 1.0) and 100% (SD 0.6) by the UED method, respectively. The UED method was the more effective in removing starch. For kale samples, starch recovery was 3.5 and 0.2% from TDF residues obtained using the AOAC and UED methods, respectively. Differences were not significant among replicate values for determination of TDF in foods by the UED method (P greater than 0.01). Preliminary studies suggest that the new method can separately determine soluble and insoluble dietary fiber. The data indicate that the UED method is more precise and accurate than the AOAC method.     

蔬菜中氯氰菊酯残留的风险评估研究

目前使用的绝大多数农药为合成农药,具有急性毒性特征,已开展的慢性评估不能完全符合实际需要,慢性评估结果容易出现过低估计风险,具有急性毒性特征的农药残留必须开展急性评估。为了推进急性评估研究,为我国食品安全监管和残留限量的制定提供技术支持,在WHO原则指导下、基于JMPR建议的方法,开展了蔬菜中氯氰菊酯残留的急性和慢性点评估技术研究。结果显示,济南、青岛和寿光三地市售的西红柿、菜椒、菜豆、茄子、豇豆和芹菜中氯氰菊酯残留摄入是安全的;虽然白菜出现了超标的个例,但99.98%的氯氰菊酯残留摄入不存在危害健康的摄入风险;即使考虑50%的总体误差以及蔬菜占总食物摄入量的比例,至少99.96%的残留摄入不存在危害健康的摄入风险。研究表明,摄入频率高的7类蔬菜中氯氰菊酯残留污染较轻,对消费者（包括孕妇、婴儿和儿童）身体健康危害很小。     

Reduction of pesticide residues on produce by rinsing

In 1997 this laboratory initiated a research program with the objective of examining the effect that rinsing of produce with tap water would have on pesticide residues. Samples were obtained from local markets and/or grown at our experimental farm. Because approximately 35% of produce from retail sources contains pesticide residues, growing and treating produce at an experimental farm had the advantage that all such samples contain pesticide residues. Pesticides were applied under normal field conditions to a variety of food crops and the vegetation was allowed to undergo natural weathering prior to harvest. The resulting samples contained field-incurred or "field-fortified" residues. This experimental design was employed to mimic as closely as possible real world samples. Crops were treated, harvested, and divided into equal subsamples. One subsample was processed unwashed, whereas the other was rinsed under tap water. The extraction and analysis method used was a multi-residue method developed in our laboratory. Twelve pesticides were included in this study: the fungicides captan, chlorothalonil, iprodione, and vinclozolin; and the insecticides endosulfan, permethrin, methoxychlor, malathion, diazinon, chlorpyrifos, bifenthrin, and DDE (a soil metabolite of DDT). Statistical analysis of the data using the Wilcoxon signed-rank test showed that rinsing removed residues for nine of the twelve pesticides studied. Residues of vinclozolin, bifenthrin, and chlorpyrifos were not reduced. The rinsability of a pesticide is not correlated with its water solubility.     

Application of gas chromatography coupled to triple quadrupole mass spectrometry for the multiresidue analysis of pesticides in olive oil

A new multiresidue method has been developed and validated for the simultaneous determination of 100 pesticide residues in olive oil. The determination of pesticide residues was carried out in only 19 min by gas chromatography coupled to tandem mass spectrometry using a triple quadrupole mass analyzer. The mass spectrometer was operated in electron ionization and the selection reaction monitoring mode was used, acquiring two or three fragmentation reactions per compound. Two extraction processes were studied, and an evaluation of the stability and sensitivity of the chromatographic system has been performed for the tested extraction procedures. The final proposed methodology was based on a liquid-liquid partition with an n-hexane/acetonitrile mixture followed by a gel permeation chromatography cleanup step. An adequate lineal relation was obtained in the studied concentration range (10-200 microg kg (-1)); the recovery values were in the range 70-110% for the two levels of concentration studied: 12 and 50 microg kg (-1). Precision values, expressed as relative standard deviation, were lower than 18% at the aforementioned spiking levels; detection limits, confirmation limits, and quantitation limits were below or equal to 1.9, 2.6, and 3.6 microg kg (-1), respectively. The developed methodology was applied to the analysis of pesticide residues in real samples of olive oil from the south of Spain.     

Refinements in acute dietary exposure assessments for chlorpyrifos.

Food pesticide residue data are used by the U.S. Environmental Protection Agency (EPA) to determine potential dietary risk from chronic and acute exposures. An acute dietary risk assessment determines the pesticide exposure resulting from a single-day consumption of food, and uses stepwise refinement of residue estimates to better judge actual exposures. All exposure refinements use estimates of the fraction of crops treated and food residues measured increasingly closer to the point of actual food consumption, without changes in the pesticide uses. Exposure distributions at all levels of data refinement were extremely right skewed. At the highest level evaluated, estimated exposures at the 99.9th percentile were 0.00087 mg/kgBW/day compared to 0.2648 mg/kgBW/day at the tolerance level for children 1-6 years, theoretically the highest-exposed population sub-group. The estimated exposure at the 99.9th percentile of the U.S. population was approximately twice the exposure at the 99th percentile and 33 times the exposure at the 90th percentile. This evaluation showed the calculated exposure at the highest tier of assessment was 300 times lower than the tolerance level assessment for children 1-6 years at the 99.9th percentile. Reduction in exposure estimates between these tiers was due to a combination of the following factors: food residue measurements in a specially designed market-basket study, government-sponsored monitoring data, probabilistic methodologies, market share information, and food processing data. This case study demonstrates that an improved understanding of the uncertainties of acute dietary exposure from pesticides is possible by using well-established statistical tools and applying them to comprehensive exposure information, including residue monitoring data, consumption data, and pesticide use information.     

Traditional food diversity predicts dietary quality for the Awajún in the Peruvian Amazon

OBJECTIVE: Our goal was to assess the potential for evaluating strengths of the Awajún traditional food system using dietary assessment, a traditional food diversity score and ranking of local foods. DESIGN: The method was used for dietary data obtained from mothers and children in the Awajún culture of the Peruvian Amazon where >90% of the dietary energy is derived from local, traditional food. Traditional food diversity scores were calculated from repeat 24-hour recalls. Group mean intakes of energy, fat, protein, iron, vitamin A and vitamin C from each food item were used to rank foods by nutrient contribution. SETTING: The study took place in six remote communities along the lower Cenepa River in the Amazonas District of Peru, South America. SUBJECTS: Dietary data were collected from 49 Awajún mothers and 34 children aged 3-6 years, representative of the six communities. RESULTS: Higher traditional food diversity was associated with greater protein, fibre, vitamin and mineral intakes when controlling for energy (partial correlations = 0.37 to 0.64). Unique sources for iron, total vitamin A and vitamin C were found in the Awajún traditional food system. CONCLUSIONS: A traditional food diversity score was a useful tool for predicting nutrient adequacy for the Awajún. Promotion of the Awajún traditional food system should focus on dietary diversity and unique nutrient-dense local foods.