Quality Control of Pesticide Residue Measurements and Evaluation of Their Results.

Pesticide residues are monitored in many countries around the world. The main aims of the programs are to provide data for dietary exposure assessment of consumers to pesticide residues and for verifying the compliance of the residue concentrations in food with the national or international maximum residue limits. Accurate residue data are required to reach valid conclusions in both cases. The validity of the analytical results can be achieved by the implementation of suitable quality control protocols during sampling and determination of pesticide residues. To enable the evaluation of the reliability of the results, it is not sufficient to test and report the recovery, linearity of calibration, the limit of detection/quantification, and MS detection conditions. The analysts should also pay attention to and possibly report the selection of the portion of sample material extracted and the residue components according to the purpose of the work, quality of calibration, accuracy of standard solutions, and reproducibility of the entire laboratory phase of the determination of pesticide residues. The sources of errors potentially affecting the measured residue values and the methods for controlling them are considered in this article.

Factors affecting the quantitative uncertainty of the estimated short-term intake. Part II-Practical examples.

The effects of the spread of residue concentrations in the samples derived from the selected supervised trials and the number of trials were studied on the magnitude and uncertainty of the short-term dietary intakes calculated with the proposed new procedure (IESTIp) and that one used currently by the FAO (Food and Agriculture Organization) and WHO (World Health Organization) Joint meeting on Pesticide Residues (JMPR) (IESTIc). The residue data of 10 pesticides were obtained from supervised trials conducted on apples and pears. The methods described in Part I were used for the calculations of the uncertainty. The results indicate that the ratio of IESTIP to IESTIc (φIESTI) is directly proportional to the ratio of the estimated maximum residue level (MRL), recommended by the JMPR; to the highest residue (HR) observed in supervised trials, and it may have a wide range depending on the particular conditions. The φIESTI becomes greater with the increase of the difference between the mrl or maximum residue limit (MRL, established by the Codex Alimentarius Commission, CAC) and HR, and becomes smaller if the difference between the large portion (LP) and unit mass (U) decreases. The φIESTI ranged between 2 and 5.1 in the 16 cases examined indicating that the IESTIp calculation method leads to higher intake estimates. The ratio of CVIESTIp and CVIESTIc ranged typically between 0.62 and 1.71. It rapidly increased up to 12 trials. For a larger number of trials, the ratio remained practically constant (1.69-1.71). The processing factor (PF) equally affects the MRL and HR values, therefore, it will not practically influence the φIESTI. The uncertainty of the estimated median residues depends on the spread and number of values in the residue datasets, which affects the uncertainty of the conversion factor (CF) and subsequently the uncertainty of the estimated IESTIp. Residue values obtained from minimum nine independent trials are required for the correct calculation of the 95% confidence intervals of the calculated median residues. The uncertainty of the analytical results directly affects the median, HR values and indirectly the calculated mrl and the MRL derived from it. Therefore, it should also be considered for the calculation of the combined uncertainty of the conversion factors. For the correct interpretation of the results of dietary exposure calculations, the upper 95% confidence limit of the short-term intake should also be considered. However, it is not the current practice of regulatory agencies or JMPR.

Factors affecting the quantitative uncertainty of the estimated short-term intake. Part I-Calculation methods.

The calculation of the combined uncertainty of the international estimated short-term intake (IESTI) of ethephon residues in apples is shown as an example. The ethephon residues in apples were reported by the Joint FAO (Food and Agriculture Organization of the United Nations)/WHO (World Health Organization) Meeting on Pesticide Residues (JMPR). The apple consumption data were taken from the IESTI (international short-term intake) calculation template used by the JMPR. The IESTI was calculated with the currently used method (case 2a) and a proposed one recommended by the EFSA (European Food Safety Authority)/RIVM (Dutch National Institute for Public Health) Scientific Workshop co-sponsored by FAO and WHO. In this example, the ratio of IESTIproposed/IESTIcurrent and their combined relative uncertainty are about 2.8, and 1.7, respectively. The larger IESTI and uncertainty obtained with the proposed equation are the consequence of calculation only with the large portion (LP) instead of its combination with unit mass, and the MRL instead of the highest residue (HR). The LP is the major contributor to the combined uncertainty. Both the calculated IESTI and its combined uncertainty depend on the actual food - pesticide residue combination, and should be calculated for each case.

Validation of a picture book to be used in a pan-European dietary survey.

OBJECTIVE: To validate a picture book for estimation of food portion sizes using two approaches: (i) 'perception' of food portions by comparison with a series of food photos; and (ii) 'conceptualization and memory', using the same photos to estimate the amount of served food one hour after self-served food portions. DESIGN: Each partner developed a country-specific picture book based on the so-called EPIC-Soft picture book. Representative and common photo series were chosen achieving approximately 25 % of the original picture book (n 23). Three portions from each photo series were randomly selected. SETTING: The study was performed within the Pilot study in the view of a Pan-European dietary survey - Adolescents, adults and elderly (PILOT-PANEU) project. SUBJECTS: A sample of adolescents and adults was recruited in five countries: Bulgaria (n 103), Finland (n 34), Germany (n 69), Hungary (n 62) and Portugal (n 77). RESULTS: Among the portions of the corresponding photo series and depending on the type of food, from 18 % (cheese) to 96 % (ratatouille) of participants chose the correct portions. In the perception study, agreement between the portions shown and reported was substantial (intraclass correlation coefficient (ICC)=0·805) and the mean difference was very low. In the memory study, agreement between the served and reported portions was lower than in the perception study (ICC=0·536). Agreement also seemed to decrease as the appearance of food on the plate differed from food in the picture. CONCLUSIONS: Overall, the picture series selected can be applied in future intake surveys to quantify foods similar to those depicted in the pictures.

Uncertainty of exposure assessment of consumers to pesticide residues derived from food consumed.

The sources of quantitative and qualitative uncertainties of the exposure of a consumer to a pesticide residue are identified. The contribution of quantifiable uncertainties of input parameters of deterministic model to the combined uncertainty of the estimated exposure is shown with detailed calculation using the pesticide residue content of food consumed during two days. The daily intakes of bifenthrin residues calculated for the 60 kg bodyweight of the reporting person are 0.00257 mg/kgbw and 0.00281 mg/kgbw for day 1 and day 2, respectively with 27-28% combined uncertainty. The major contributors were fruits and whole meal bread. The contribution of the individual steps to the combined uncertainty depends on the particular food item. In general, the variability of recipes, estimation of the mass of consumed food, sampling, processing of raw commodities and analysis of pesticide residues influenced most, in decreasing order, the combined uncertainty of the estimated daily exposure.