Analytical methods for residues

For certain naturally occurring nontoxic a.i., an enforcement is not sensible (e.g., lecithin, rape seed oil). Analytical methods for residues in soil are not necessary if the DTgo values of the a.i. and relevant metabolites are less than 3 days (e.g., fosetyl), because in general, the results from residue analyses are not meaningful if the a.i. is rapidly degraded. 

Analytical Methods for Residues of Pesticides in Foodstuffs, fifth edition, Rijswiik (1988) amended by Analytical Methods for Pesticide Residues in Foodstuffs, ed. P. van Zoonen, sixth edition. General Inspectorate for Health Protection, The Hague (1996). 

Committee for Analytical Methods for Residue of Pesticides and Veterinarian Products in Foodstuffs by Headspace Method, of MAFF, Report by the Panel of the Determination of Dithiocar-bamate Residues, Ana/yit, 106,781 (1981). 

Panel 2 of the Committee for Analytical Methods for Residues of Pesticides and Veterinary Products in Foodstuffs of the Ministry of Agriculture, Fisheries and Food (1976) Analyst 101 386. 

Analytical methods for residues in food Consumer safety... 

Until a more detailed metabolic profile of PBO has been established, the analytical method for residue assessment is based on the amount of the parent compound (PBO) that is present. This will give a reasonable approximation of the level in milk. In the case of crops, acid hydrolysis to methylenedioxy benzyl alcohol can be used to quantitate the majority of the residues present. 

Analytical Methods for Residues. After the marker residue and target tissue have been identified and a tolerance level or Rm has been set, the sponsor develops determinative and confirmatory methods for the marker residue at the tolerance. The determinative method must be practical and rugged to be useful for routine surveillance monitoring of residues in meat in USDA field laboratories. The confirmatory method is one in which the marker residue is determined unequivocally so that the identity of an above tolerance residue can be supported in a court of law. Methods that are capable of this level of specificity often employ mass spectrometry in one form or another. 

The TMDI is compared to the ADI. The TMDI must not result in exposures in excess of the ADI. In the example above, the TMDI represents 95% of the ADI. While a specific study and its associated analytical method may provide the data used to establish the marker total ratio, there is no unbreakable link between the MRLs and any specific analytical method for residue monitoring. 

B. Residue Testing (Metabolism and residue kinetics, Routine analytical method for the detection of residues)... 

Fukuhara K, Takeda M, Uchiyama M. 1977. [Studies on analysis of pesticide residues in foods (XXV) Analytical method for endosulfan in crops.] ShokuhinEiseigakuZasshi 18 149-153. (Japanese)... 

Handbook of Residue Analytical Methods for Agrochemicals. 2003 John Wiley Sons Ltd. 

Reviews and checks out analytical methods for pesticides submitted by registrants Monitors residues in imported and domestic food, including processed food Monitors residues in meat and poultry Conducts market basket surveys Monitors pesticides in fish and wildlife... 

Assessment of residue analytical methods for crops, food, feed, and environmental samples the approach of the European Union... 

Commission Directive 96/46/EC of 16 July 1996, amending Annex II to the Directive 91/414/EEC, is the basis for the assessment of residue analytical methods for crops, food, feed, and environmental samples." Provisions of this Directive cover methods required for post-registration control and monitoring purposes but not data generation methods. Because it is necessary to provide applicants as precisely as possible with details on the required information, the guidance document S ANCO/825/00 rev. 6 dated 20 June 2000 (formerly 8064/VI/97 rev. 4, dated 5 December 1998)" was elaborated by the Commission Services in cooperation with the Member States. 

Owing to the complexity of multi-residue methods for products of animal origin, it is not possible to outline a simple scheme however, readers should refer to methods described in two references for detailed guidance (Analytical Methods for Pesticides in Foodstuffs, Dutch method collection and European Norm EN 1528. ) There is no multi-method specifically designed for body fluids and tissues. The latter matrix can be partly covered by methods for products of animal origin. However, an approach published by Frenzel et al may be helpful (method principle whole blood is hemolyzed and then deproteinized. After extraction of the supernatant, the a.i. is determined by GC/MS. The LOQ is in the range 30-200 ag depending on the a.i.). 

Validation of the analytical methods for food of animal origin has to be performed with milk, egg, meat, and fat. The latter is required only if log Pqav is >3 and metabolism studies indicate significant residues in fat, because in this case it is likely that an MRL will be set. Other tissues such as kidney or liver must be validated only if an MRL is set or proposed for these tissues. The issue of the general necessity of analytical methods for food of animal origin is not addressed in Directive 96/46/EC or SANCO/825/00. At this moment, the Working Group Pesticide Residues proposes an MRL on a case-by-case basis. However, a pragmatic approach is presented in SANCO/825/00. 

According to Directive 96/68/EC, an analytical method for the determination of residues in food of animal origin is not required when metabolism study in animals is not required. On the other hand, according to Point 6.4 of the Directive, where a feeding study is required, an analytical method for the determination of residues in products of animal origin must be submitted. In other cases, the requirement for an analytical method depends on the establishment of an MRL for food commodities of animal origin. 

Analytical methods for the determination of residues in body fluids and tissues must be submitted only if the a.i. is classified as toxic or highly toxic. The method has to be validated only at the LOQ in general blood 0.05 mgL and tissues 0.1 mgkg (meat or liver, if not investigated under food of animal origin, see Section 4.2.1). 

The conditions for validation of an analytical method for the determination of residues in air are the same as the requirements given in Section 4.2.5. 

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