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GB 23200.62-2016 English PDF

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GB 23200.62-2016: Food safety national standard -- Determination of fulvic acid residues in foodstuffs by gas chromatography-mass spectrometry
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Standard similar to GB 23200.62-2016

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Basic data

Standard ID GB 23200.62-2016 (GB23200.62-2016)
Description (Translated English) Food safety national standard -- Determination of fulvic acid residues in foodstuffs by gas chromatography-mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 14,124
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 2459-2010
Regulation (derived from) State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of 2016
Issuing agency(ies) National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration

GB 23200.62-2016: Food safety national standard -- Determination of fulvic acid residues in foodstuffs by gas chromatography-mass spectrometry


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Food safety national standards - Determination of fulvic acid residues in foodstuffs by gas chromatography - mass spectrometry National Standards of People's Republic of China GB Instead of SN/T 2459-2010 National standards for food safety Determination of fenvalerate residues in food Gas chromatography - mass spectrometry National food safety standards- Determination of flumiclorac-pentyl residue in foods Gas chromatography-mass spectrometry 2016-12-18 Release.2017-06-18 Implementation National Health and Family Planning Commission of the People 's Republic of China Issued by the Ministry of Agriculture of the People 's Republic of China State Administration of Food and Drug Administration

Foreword

This standard replaces SN/T 2459-2010 "Determination of fenvalerate residues in food for import and export by gas chromatography-mass spectrometry". Compared with SN/T 2459-2010, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name and scope of the "import and export food" to "food"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 2459-2010. National standards for food safety Determination of fulvic acid residues in foodstuffs by gas chromatography - mass spectrometry

1 Scope

This standard specifies the method for the determination of fenvalerate residues in food by gas chromatography-mass spectrometry. This standard applies to corn, celery, apples, peanuts, tea, beef, chicken liver, fish, honey, soy and milk in the fluoride The amount of detection and confirmation, other food can refer to the implementation.

2 normative reference documents

The following documents are indispensable for the application of this document. For dated references, only the dated edition applies to this article Pieces. For undated references, the latest edition (including all modifications) applies to this document. GB 2763 National Standard for Food Safety - Maximum Residue Limit of Pesticides in Foodstuffs GB/T 6682 Analytical laboratory water specifications and test methods

3 principle

The residual fluoroacetic acid in the sample was extracted with ethyl acetate or acetonitrile. The extracted organic phase was evaporated to dryness and the residue was extracted with ethyl acetate-cyclohexane (1 1) was dissolved and purified by gel permeation chromatography (GPC). The eluate was evaporated to dryness, and the ion detection was selected by gas chromatography-mass spectrometry. External standard method.

4 reagents and materials

Unless otherwise specified, all reagents are of analytical grade and water is in accordance with the primary water specified in GB/T 6682. 4.1 Reagents 4.1.1 Acetone (C3H6O). Pesticide level. 4.1.2 Ethyl acetate (C4H8O2). 4.1.3 Cyclohexane (C6H12). 4.1.4 Acetonitrile (CH3CN). liquid chromatography grade. 4.1.5 n-hexane (C6H14). 4.1.6 Sodium chloride (NaCl). 4.1.7 anhydrous sodium sulfate. at 650 ℃ for 4 h, stored in a sealed container in reserve. 4.2 solution preparation 4.2.1 Acetonitrile saturated n-hexane. 4.2.2 n-hexane saturated acetonitrile. 4.2.3 Ethyl acetate - cyclohexane (1 1, V/V). Mix the ethyl acetate and cyclohexane in equal volume and mix. 4.2.4 sodium chloride solution..200 g/L, take.200 gNaCl, constant volume to 1 L. 4.3 standards 4.3.1 Fenvalerate standard. English name. flumiclorac-pentyl, CAS. 87546-18-7, purity ≥ 99%. 4.4 standard solution preparation 4.4.1 standard solution of fenvalerate. accurately weighed the appropriate amount of fluoroacetic acid standard, formulated with acetone 100 μg/mL standard reserve liquid. 4.4.2 Fenvalerate standard intermediate solution. 1 μg/mL. Accurately absorb 1 mL of the standard stock solution into a 100 mL volumetric flask with acetone Constant volume to the scale, the solution stored at 0 ~ 4 ℃. 4.4.3 Matrix standard working solution. If necessary, use a blank sample according to the sample treatment steps of the extract, with different concentrations of the base Quality standard working solution, matrix standard working solution to be used with the current distribution. 4.5 Materials 4.5.1 Gel Permeation Column. The filler is S-X3 BioBeads, 22g. 4.5.2 anhydrous sodium sulfate column. in the 150 mm × 10 mm (diameter) column, followed by adding absorbent cotton and 5 cm anhydrous sodium sulfate.

5 instruments and equipment

5.1 Gas Chromatography-Mass Spectrometer. Electronically bombarded ion source. 5.2 Analysis of the balance. the amount of 0.0001 g. 5.3 Analysis of balance. 0.01 g. 5.4 Homogenizer. 5.5 Centrifuge. 5.6 Rotary evaporator. 5.7 gel permeation chromatography (hereinafter referred to as GPC). 5.8 Scroll Mixer. 5.9 centrifuge tube, 50 mL, polypropylene.

6 Preparation and storage of samples

During the sample preparation operation, it is necessary to prevent the sample from being contaminated or the change in the content of the residue. 6.1 fruit, vegetables Take about 500 g of the sample, crush with a pulverizer, into a clean container as a sample, sealed and marked, stored in -18 ℃ refrigerator. 6.2 nuts Take about 500 g, crushed with a pulverizer, into a clean container as a sample, sealed and well marked, stored in the refrigerator at 4 ℃. 6.3 grain, tea Take about 500 g of the sample, crushed into a whole by a pulverizer through a 20 mesh sieve, into a clean container as a sample, sealed and marked, Store at room temperature. 6.4 Meat and aquatic products Take about 500 g of the sample, crush with a pulverizer, into a clean container as a sample, sealed and marked, stored in -18 ℃ refrigerator. 6.5 honey Take a representative sample of about 500 g, the amorphous sample will be forced to stir evenly, there are crystallization of the sample can be sealed after the sample cap, Placed in a water bath of not more than 60 ℃, until the sample all dissolved and stir well, quickly cooled to room temperature. The prepared sample is packed in a clean container Sealed and well marked, room temperature preservation. 6.6 milk Take about 500 g sample, mix well, install clean container as sample, seal and make sure, save at -18 ℃. Note. The above sample sampling site according to GB 2763 Appendix A implementation.

7 Analysis steps

7.1 Extraction 7.1.1 Fruits and vegetables Weigh the sample about 10 g (accurate to 0.01 g) in a 50 mL centrifuge tube, add 10 g of anhydrous sodium sulfate and 20 mL of ethyl acetate,.20000 r/min Homogenized extraction 2 min, 4000 r/min centrifugal 10 min, the upper organic phase through the anhydrous sodium sulfate column into the heart of the bottle. The residue was washed with 20 mL Ethyl acetate repeated extraction, centrifugal filtration, the combined secondary extract, the extract in 45 ℃ water bath with a rotary evaporator concentrated to near dry, To be purified by GPC. 7.1.2 tea, grain, soybeans, peanuts Weigh the sample about 10 g (accurate to 0.01 g) in 150 mL with a triangular flask, add 50 mL of acetonitrile,.20000 r/min homogeneous extraction 2 min, The upper organic phase is filtered into the separatory funnel. The residue was extracted once again with 50 mL of acetonitrile and filtered, and the combined extracts were separated in a separatory funnel. 7.1.3 Livestock, poultry, aquatic products Weigh the sample about 10 g (accurate to 0.01 g) in a 50 mL centrifuge tube, 10 g sodium chloride, mix, add 20 mL acetonitrile,.20000 r/min Homogenized 2 min, centrifuged at 4000 r/min for 5 min. The upper organic phase was passed through an anhydrous sodium sulfate column and transferred to a separatory funnel. And then with 20 mL of acetonitrile each time The residue was extracted twice in the same manner as described above, and the organic phases were combined in a separatory funnel. 7.1.4 honey Weigh 10 g (accurate to 0.01 g) honey sample in 150 mL Erlenmeyer flask, add 20 ml of water to dissolve, shake for 30 min on a flat shaker, Transferred to 250ml separatory funnel, and then were 30 mL of water and 50 mL of ethyl acetate in two times the original prune bottle, are transferred into the separatory funnel, vibration Shake 2min, standing stratification (if the occurrence of emulsification, the upper layer and the emulsion layer can be centrifuged at 4000r/min 5min, take the upper transfer into the liquid Funnel), the organic phase was passed through an anhydrous sodium sulfate column in a heart-shaped bottle. The lower aqueous phase was added twice every 20 ml of ethyl acetate, gently shaken for 1 min, Placed in the heart of the bottle, in 45 ℃ water bath with a rotary evaporator concentrated to near dry, to be GPC purification. 7.1.5 milk Weigh 10 g (accurate to 0.01 g) milk sample in 50 mL stoppered centrifuge tube, add 20 mL of acetonitrile, vortex for 1 min, White, 4000 r/min centrifugal 5 min, the supernatant filter into the heart of the bottle, in the 45 ℃ water bath on the vacuum slowly evaporate to about 10 mL, The solution was transferred to a 250 mL separatory funnel and 10 mL of sodium chloride solution was added, mixed, 20 mL of ethyl acetate was added, shaken for 2 min, allowed to stand Layered. The ethyl acetate layer was transferred to a 150 mL heart flask and the lower aqueous phase was further added with 20 mL of ethyl acetate solution to extract the aqueous phase, Ester layer into the heart of the bottle, in 45 ℃ water bath rotary evaporator concentrated to near dry, to be GPC purification. 7.2 Purification 7.2.1 livestock, poultry, aquatic products, peanuts, grain, tea, soybeans The organic phase solution obtained in 7.1.2 and 7.1.3 was added with 40 ml of acetonitrile saturated n-hexane and shaken for 2 min. The layers were allowed to stand and the acetonitrile layer was transferred Heart-shaped bottles, n-hexane layer each time again with n-hexane saturated acetonitrile 15 mL wash twice, acetonitrile layer into the same heart bottle, in the 45 ℃ water bath Vacuum Rotate to dry. With ethyl acetate - cyclohexane volume 10 mL, to be GPC purification. 7.2.2 fruit, vegetables, honey, milk The residue obtained by dissolving 7.1.1, 7.1.4 and 7.1.5 with ethyl acetate-cyclohexane was fixed at 10 mL and operated as follows. 7.2.3 Gel permeation chromatography purification 7.2.3.1 Conditions A) Purification column. 400 mm (length) × 25 mm (inner diameter), built with BIO-Beads S-X3 packing or equivalent. B) Mobile phase. ethyl acetate-cyclohexane (1 1). C) Flow rate. 4.7 mL/min. D) Injection volume. 5 mL. E) Start collection time. 9.5 min. F) End of collection time. 14.0 min. 7.2.3.2 Purification The solutions obtained in 7.2.1 and 7.2.2 were injected with 5 mL of the sample and purified by gel permeation chromatography. A fraction of 9.5 to 14 min was collected in a heart And evaporated to dryness in a water bath at 45 ° C, fixed to 1 mL with acetone and determined by gas chromatography-mass spectrometry. 7.3 Preparation of blank matrix solution Weigh the negative samples of the various substrates 10 g, according to 7.1 and 7.2 operation. 7.4 determination 7.4.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. DB-5MS, 30 m (length) × 0.25 mm (inner diameter) × 0.25 μm (film thickness) or equivalent. B) Column temperature programmed..200 ° C (for 1 min) and ramp up to 280 ° C (for 12 min) at a rate of 10 ° C/min. C) Inlet temperature. 280 ° C. D) Carrier gas. helium, purity 99.999%. E) Carrier gas flow rate. constant current mode 1 mL/min. F) Injection mode. no shunt. G) Injection volume. 2 μL. H) Interface temperature. 280 ° C. I) ion source. electron bombardment source (EI). J) Ionization voltage. 70eV. K) ion source temperature. 230 ° C. L) Detection method. SIM. M) Select the ion and relative abundance. see Table 1. Table 1 Select the ion and relative abundance The quantified ion is quantified by the measured component Select ion (m/z) 423 308 318 280 Relative abundance (%) 100 49 26 12 7.4.2 Quantitative determination The volume of the sample solution and the standard working fluid and so on. The actual application of the standard working fluid and the sample to be measured, the reaction of fluoroacetic acid Values should be within the linear range of the instrument. Under the above conditions of gas chromatography-mass spectrometry, the retention time of fenvalerate was about 15.9 min. standard See Appendix A for gas chromatography-mass spectrometry. 7.4.3 Qualitative determination When the sample is measured, if the mass retention time of the detected mass is consistent with that of the standard sample, and the sample spectrum after subtracting the background , The relative abundance of the qualitative ions is close to the standard solution obtained under the same conditions as the standard solution spectrum, the error does not exceed the provisions of Table 2 Range, you can determine the existence of the corresponding sample in the sample. Table 2 The maximum allowable error of relative ion abundance when qualitative confirmation Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50% 7.5 blank test Except for the same conditions and procedures as described above.

8 results are calculated and expressed

Use the chromatographic data processor or according to formula (1) calculation, the calculation results need to deduct the blank value. X = MAs VcA  (1) Where. X - Residue of fenvalerate in milligrams per kilogram (mg/kg); A - the peak area of fenvalerate in the sample solution; in square millimeters (mm2); C - the concentration of fenvalerate in the standard solution, in micrograms per milliliter (μg/mL); V - the final volume of the sample solution in milliliters (mL); As - the peak area of fenvalerate in standard solution; in square millimeters (mm 2); M - the amount of sample represented by the final sample, in grams (g). Note. The result of the calculation shall be deducted from the blank value. The result of the measurement shall be expressed as the arithmetic mean of the parallel measurement, and two valid digits shall be retained.

9 precision

9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with Appendix C requirements. 9.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with Appendix D requirements. 10% limit and recovery rate 10.1 Quantitation limits The limit of quantification of fenvalerate is 0.005 mg/kg. 10.2 Recovery rate When the levels were 0.005 mg/kg, 0.01 mg/kg, 0.05 mg/kg, the addition rates for the addition of fenvalerate were given in Appendix B.

Appendix A

(Informative) Gas Chromatography - Mass Spectrometry of Fluoroally Oxalic Acid Standard Figure A.1 Gas Chromatography-Mass Spectrometry (TIC) of Fenvalerate Standards 1-fluoro-oxalic acid Figure A.2 Full scan of the fluoroacetic acid standard

Appendix B

(Informative) Sample concentration and recovery of the experimental data Table B.1 Experimental data on the concentration and recovery of the sample Substrate addition level/(mg/kg) Recovery/(%) corn 0.005 71.6 ~ 102.0 0.010 78.8 ~ 94.1 0.050 85.6 ~ 101.0 celery 0.005 79.6 ~ 96.8 0.010 82.2 to 100.3 0.050 81.8 ~ 100.2 apple 0.005 77.6 ~ 99.0 0.010 75.4 to 96.3 0.050 81.2 ~ 95.6 peanut 0.005 77.2 ~ 94.2 0.010 78.3 to 96.7 0.050 80.0 ~ 97.8 tea 0.005 79.8 ~ 99.0 0.010 79.5 to 97.2 0.050 79.4 to 97.0 beef 0.005 76.4 to 99.2 0.010 79.6 ~ 95.3 0.050 81.2 ~ 99.4 Chicken liver 0.005 77.4 ~ 93.6 0.010 76.1 to 98.2 0.050 82.2 ~ 94.8 0.005 79.8 ~ 97.0 0.010 79.2 ~ 100.6 0.050 82.6 ~ 99.2 honey 0.005 81.4 ~ 97.6 0.010 86.8 ~ 101.8 0.050 84.4 to 100.2 Soybeans 0.005 77.2 ~ 94.2 0.010 78.3 to 96.7 0.050 80.0 ~ 97.8 milk 0.005 80.4 to 98.2 0.010 82.6 ~ 92.4 0.050 85.6 ~ 95.8

Appendix C

(Normative appendix) Laboratory repeatability requirements Table C.1 Laboratory repeatability requirements Measured component content Mg/kg Precision 0.001 36 > 0.01 > 1 14

Appendix D

(Normative appendix) Inter-laboratory reproducibility requirements Table D.1 Inter-laboratory reproducibility requirements Measured component content Mg/kg Precision 0.001 54 > 0.01 > 1 19

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