Analytical Methods for Residual Compositional Substances of Agricultural Chemicals, Feed Additives, ∗ and Veterinary Drugs in Food
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Analytical Methods for Residual Compositional Substances of Agricultural Chemicals, Feed Additives, ∗ and Veterinary Drugs in Food Department of Food Safety Ministry of Health, Labour and Welfare ∗ This document is an annex of the Director Notice about Analytical Methods for Residual Compositional Substances of Agricultural Chemicals, Feed Additives, and Veterinary Drugs in Food (Syoku-An No.0124001, January 24, 2005. Final amendments were made on May 26, 2006.). 1 General Rules 1. Terminology (1) The term “Substances to be analyzed” refers to substances that should be analyzed using the analytical methods stipulated in this document. The relevant compositional substances of agricultural chemicals, feed additives or veterinary drugs (hereinafter referred to as “agricultural chemicals”) (including substances formed through chemical reactions with these substances) and any related substances (such as their salts, or optical isomers) are listed in the Tables in item 6 (1), item 7 (1), and item 9 (1), Section A General Compositional Standards for Food, Part 1 Food under the Specifications and Standards for Food, Food Additives, Etc.(Ministry of Health and Welfare Notification No. 370, 1959; hereinafter referred to as “the Notification No. 370”) (2) The term “Analytical Value” means a value taken from a food listed in the Notification No. 370 that will be compared with the maximum residue limit of the substances to be analyzed of the agricultural chemicals. (3) The term “Nuts and Seeds” refers to oil seeds, nuts, cacao beans, and coffee beans. (4) The term “Limit of quantitation” refers to the minimum amount or concentration of a substance to be analyzed from a sample with which the amount or concentration of the target substance can be determined. For chromatography, the substances to be analyzed which show the ratio of S (peak height) / N (baseline noise) = 10 are represented as the concentrations of compositional substances of agricultural chemicals. (5) The word “Type” refers to the source of the testing method used for analysis, which is classified as follows: A: Official analytical methods stipulated by Ministerial Ordinance Concerning Composiotional Standards, Etc. for Milk and Milk Products (Ministry of Health and Welfare Ordinance No. 52, 1951), Notification No. 370 and announcement (excluding type C) B: Analytical methods stipulated by the governmental organizations, etc., of foreign countries (excluding Type A) C: Analytical methods established by the investigational commission of experts in Japan D: Analytical methods described in the references (excluding types A to C) 2. Reagents Reagents used for analyses by the testing methods pertain specifically to those listed in this Notice in Section C Reagents, Part II Food Additives in the Notification No. 370 or the following attachment. Reagents designated as “special grade” in this Notice must meet the requirements for “special grade” specified in the Japan Industrial Standards for the reagents. 3. Samples Unless otherwise specified, a sample to be used for analysis by the method stipulated in this document should be prepared according to the following steps. 2 (1) For grains, beans, nuts and seeds, pulverize a sample into particles that can be passed through a 420-μm standard sieve. (2) For fruits, vegetables and herbs, precisely weigh out approximately 1 kg to be used as the sample, cut into small pieces, and homogenize. If necessary, add a sufficient amount of water during homogenization. (3) For tea and hops, pulverize a sample into particles that can be passed through a 420-μm standard sieve. For tea types other than green powdered tea, homogenize the pulverized samples. (4) For spices, follow the sample preparation method for “nuts and seeds” or “fruits” according to the shape of the sample. (5) For animal muscle, remove the fat from the sample as much as possible, cut into small pieces, and homogenize. (6) For animal fat, remove the muscle from the sample as much as possible, cut it into small pieces, and homogenize. (7) For animal liver, kidney, or other edible offal, cut the sample into small pieces and homogenize. (8) For milk and honey, homogenize a sample by thoroughly mixing. (9) For fish, cut edible parts into small pieces and homogenize. (10) For shellfish, remove the shell from the sample, cut the meat into small pieces, and homogenize. (11) For crustaceans, cut the whole into small pieces for a small sample or cut into small pieces after removing the outrmost shell for a large sample, and homogenize.. (12) For eggs, use only the white and york of the sample. Mix thoroughly, and homogenize the mixture (except if a maximum residue limit in the white or york is established). 4. Precautions during Analysis (1) To perform an analysis using a method not stipulated in this Notice, the method should have an accuracy, precision or limit of quantitation comparable to or higher than that of the corresponding analytical method stipulated in this Notice, and specificity. (2) To obtain an analytical value, the number of decimal places of the measured value should be one more than that of the corresponding maximum residue limit. Round off the measured value to the last decimal place of the maximum residue limit. 3 (Attachment) Acrylamide copolymer bonded glycerylpropylsilanized silica gel mini column (360 mg) 360 mg of acrylamide copolymer bonded glycerylpropylsilanized silica gel is packed in a polyethylene column tube with an inner diameter of 8 to 9 mm or a column with comparable separation efficiency. Acetonitrile Use a rotary vacuum evaporator on 300 mL of acetonitrile to concentrate to the point of dryness. Dissolve the residue in 5 mL of n-hexane. For analysis, inject 5 μL of the solution into a gas chromatograph equipped with an electron capture detector. Peaks other than that of n-hexane in the resulting chromatogram should be as high as or lower than the peaks of γ-BHC at 2 x 10-11 g. Acetone Use a rotary vacuum evaporator on 300 mL of acetone to concentrate to the point of dryness. Dissolve the residue in 5 mL of n-hexane. For analysis, inject 5 μL of the solution into a gas chromatograph equipped with an electron capture detector. Peaks other than that of n-hexane in the resulting chromatogram should be as high as or lower than the peaks of γ-BHC at 2 x 10-11 g. Aminopropylsilanized silica gel mini column (360 mg) 360 mg of aminopropylsilanized silica gel is packed in a polyethylene column tube with an inner diameter of 8 to 9 mm or a column with comparable separation efficiency. Aminopropylsilanized silica gel mini column (500 mg) 500 mg of aminopropylsilanized silica gel is packed in a polyethylene column tube with an inner diameter of 8 to 9 mm or a column with comparable separation efficiency. Aminopropylsilanized silica gel mini column (1,000 mg) 1,000 mg of aminopropylsilanized silica gel is packed in a polyethylene column tube with an inner diameter of 12 to 13 mm or a column with comparable separation efficiency. Sodium sulfite Sodium sulfite (special grade) Potassium sulfite Potassium sulfite (special grade) Argon Purity of 99.998 v/v% or higher Isopropylether Isopropylether (special grade) Ethanol Use a rotary vacuum evaporator on 300 mL of ethanol to concentrate to the point of dryness. Dissolve the residue in 5 mL of n-hexane. For analysis, inject 5 μL of the solution into a gas chromatograph equipped with an electron capture detector. Peaks other than that of n-hexane in the resulting chromatogram should be as high as or lower than the peaks of γ-BHC at 2 x 10-11 g. Ethylsilanized silica gel mini column (1,000 mg) 4 1,000 mg of ethysilanized silica gel is packed in a polyethylene column tube with an inner diameter of 12 to 13 mm or a column with comparable separation efficiency. 3 mol/L Ether solution of ethylmagnesiumbromide 3 mol/L Ether solution of ethylmagnesiumbromide Ethylenediamine-N-propylsilanized silica gel mini column (500 mg) 500 mg of ethylenediamine-N-propylsilanized silica gel is packed in a polyethylene column tube with an inner diameter of 8 to 9 mm or a column with comparable separation efficiency. Ether Use a rotary vacuum evaporator on 300 mL of ether to concentrate to the point of dryness. Dissolve the residue in 5 mL of n-hexane. For analysis, inject 5 μL of the solution into a gas chromatograph equipped with an electron capture detector. Peaks other than that of n-hexane in the resulting chromatogram should be as high as or lower than the peaks of γ-BHC at 2 x 10-11 g. Ferrous chloride Ferrous chloride (special grade) Sodium chloride Sodium chloride (special grade). If the reagent is found to include any substance that may interfere with the analysis of substances to be analyzed from agricultural chemicals, wash with a solvent such as n-hexane before use. Basic alumina mini column (1,710 mg) 1,710 mg of basic alumina is packed in a polyethylene column tube with an inner diameter of 8 to 9 mm or a column with comparable separation efficiency. Guanidine hydrochloride Guanidine hydrochloride (special grade) Pyridine hydrochloride Pyridine hydrochloride (special grade). If the reagent is found to include any substance that may interfere with the analysis of target compositional substances from agricultural chemicals, wash with a solvent such as n-hexane before use. Octadecylsilanized silica gel mini column (360 mg) 360 mg of octadecylsilanized silica gel is packed in a polyethylene column tube with an inner diameter of 8 to 9 mm or a column with comparable separation efficiency. Octadecylsilanized silica gel mini column (500 mg) 500 mg of octadecylsilanized silica gel is packed in a polyethylene column tube with an inner diameter of 8 to 9 mm or a column with comparable separation efficiency.