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GB 23200.52-2016 English PDF

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GB 23200.52-2016: Food safety national standard -- Determination of residues of cyclic azole in food by gas chromatography-mass spectrometry
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GB 23200.52-2016English219 Add to Cart 3 days [Need to translate] Food safety national standard -- Determination of residues of cyclic azole in food by gas chromatography-mass spectrometry Valid GB 23200.52-2016

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Standard similar to GB 23200.52-2016

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Basic data

Standard ID GB 23200.52-2016 (GB23200.52-2016)
Description (Translated English) Food safety national standard -- Determination of residues of cyclic azole in food by gas chromatography-mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 11,172
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 2235-2008
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 23200.52-2016: Food safety national standard -- Determination of residues of cyclic azole in food by gas chromatography-mass spectrometry


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Food safety national standard - Determination of residues of cyclic azole in food by gas chromatography - mass spectrometry National Standards of People's Republic of China GB Instead of SN/T 2235-2008 National standards for food safety Determination of Cyclosine Residue in Food Gas chromatography - mass spectrometry National food safety standards- Determination of cyprodinil 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 2235-2008 "Determination of azolethine residues in food for import and export by gas chromatography-mass spectrometry". This standard compared with SN/T 2235-2008, 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 2235-2008. National standards for food safety Determination of residues of cyclic azole in food by gas chromatography - mass spectrometry

1 Scope

This standard specifies the method of gas chromatography-mass spectrometry detection and confirmation of azoxicillin residues in food. This standard applies to rice, soybeans, small cabbage, sweet peas, pears, citrus, peanuts, tea, beef, chicken, shrimp, honey Detection and confirmation of residual residues of azoxystrobin residues, 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 azoxystrobin in the sample was extracted with n-hexane-acetone (1 1, by volume), washed with gel permeation column and propanesulfonylsilane Base silica gel cation exchange column purification, gas chromatography - mass spectrometry detection and confirmation, external standard method quantitative.

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 n-hexane (C6H14). chromatographic purity. 4.1.2 Acetone (C3H6O). Chromatographic pure. 4.1.3 Cyclohexane (C6H12). Chromatographic Purification. The 4.1.4 ethyl acetate (C4H8O2). chromatography pure. 4.1.5 Methanol (CH3OH). Chromatographic Purification. 4.1.5 Ammonia (NH3 · H2O). Analytical purity. 4.1.7 Hydrochloric acid (HCl). Analytical purity. The 4.1.8 Sodium chloride (NaCl). Analytical purity. 4.1.9 anhydrous sodium sulfate (Na2SO4). analysis of pure, 650 ℃ burning 4h, in the dryer to cool to room temperature, stored in a sealed bottle in reserve. 4.2 solution preparation 4.2.1 0.1 moL/L hydrochloric acid solution. the amount of 9 mL of hydrochloric acid, add appropriate amount of water diluted to 1000 mL. 4.3 standards 4.3.1 Cyprodinil standard substance. purity > 99%, molecular formula. C14H15N3, molecular weight. 225.3 CAS Registry Number. 121552-61-2. 4.4 standard solution preparation 4.4.1 azoxystine standard solution. accurately weighed the appropriate amount of azoxicillin amine standard material, with acetone dosing concentration of 100 g/mL standard Stock solution. According to the need to use acetone diluted to the appropriate concentration of standard working fluid. The standard stock solution is stored in 0 ℃ ~ 4 ℃ refrigerator, valid period For 12 months, the standard working fluid in 0 ℃ ~ 4 ℃ refrigerator to save, valid for 6 months. 4.5 Materials 4.5.1 Propanesulfonylsilyl Silicone Cation Exchange Column. 3 mL, 500 mg or equivalent.

5 instruments and equipment

5.1 Gas Chromatography-Mass Spectrometer. Equipped with an electron impact source (EI). 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Centrifuge. speed greater than 5 000 r/min. 5.4 nitrogen blowing instrument. 5.5 Rotary evaporator. 5.6 Homogenizer. 5.7 solid phase extraction device. 5.8 Multifunctional food mixers. 5.9 Shredder. 5.10 gel permeation chromatography. 5.11 Vortex Mixer.

6 Preparation and storage of samples

6.1 Preparation of the sample 6.1.1 tea, grain category Approximately 500 g of the representative sample was ground and pulverized by a pulverizer and passed through a 2.0 mm round hole sieve, mixed and sealed in a clean container. mark. 6.1.2 Vegetables, fruits and nuts Replace the sample of about 500 g, chopped, the multi-functional food mixer fully mashed evenly, into a clean container sealed, marked the standard Remember. 6.1.3 Livestock, poultry, aquatic products Replace the sample of about 500 g, chopped, with a multi-functional food mixer fully mashed uniform, sealed into a clean container, marked mark. 6.1.4 Bee products To replace the sample about 500 g, the crystallization of the sample will be forced to stir evenly, the crystallization of the sample can be sealed after the sample cap, Placed in a water bath of not more than 60 ° C warm, and so the sample all melted and then stir, quickly cooled to room temperature. In the melting must pay attention to prevent water Points volatile. Sealed in a clean container and marked with a mark. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage Tea, cereals, bee products, nuts and other samples stored below 4 ℃; vegetables, fruits, livestock, poultry, aquatic products such as samples at -18 ℃ Save the following. In the process of sample preparation, should prevent the sample contamination or the occurrence of azoxystine residues in the amount of change.

7 Analysis steps

7.1 Extraction 7.1.1 Shrimp Weigh 20 g (accurate to 0.01 g) sample, add 10 mL of water to mix, add 30 mL of n-hexane - acetone (1 1, volume ratio) Solution, homogenized at 10 000 r/min for 0.5 min, 5 g sodium chloride was added, shaken and centrifuged at 4 000 r/min for 3 min. Learn the upper layer The solution was mixed with 30 mL of n-hexane-acetone (1 1, volume ratio) mixture, and the mixture was extracted once again. The organic phase was concentrated in a 45 ° C water bath under reduced pressure to near dryness. Accurately add 10.0 mL of cyclohexane-ethyl acetate (1 + 1, by volume) to dissolve the residue, For gel chromatography. 7.1.2 honey Weigh 20 g (accurate to 0.01 g) sample, add 20 mL of water to mix, add 30 mL n-hexane - acetone (1 1, volume ratio) vortex Spin mixed for 1 min, add 5 g of sodium chloride, shake, and centrifuged at 4 000 r/min for 3 min. Absorb the upper organic phase in the concentrated bottle, the residue Was added 30 mL of n-hexane-acetone (1 1, volume ratio) mixed solution, repeated extraction once, combined with the upper organic phase, in a 45 ° C water bath Concentrated to near dryness. Accurately add 10.0 mL of cyclohexane-ethyl acetate (1 + 1, volume ratio) to dissolve the residue for gel chromatography. 7.1.3 rice, soybeans, peanuts, tea, small cabbage, sweet peas, pears, citrus, beef, chicken Weigh 5 g (tea weighing 2 g) (accurate to 0.01 g) sample, add 5 mL of water to mix (tea, rice and peanuts need to place 0.5 h) Add 15 mL of n-hexane - acetone (1 1, volume ratio) mixed solution, 10 000 r/min homogenization 0.5 min, adding 5 g sodium chloride, shake And centrifuged at 4 000 r/min for 3 min. Absorb the upper organic phase in the concentrated flask, add 15 mL of the hexane - acetone (1 1, Volume ratio) mixed solution, repeated extraction once, combined with the upper organic phase, in a water bath at 45 ℃ under reduced pressure to near dry. Accurately add 10.0 mL Cyclohexane-ethyl acetate (1 + 1, by volume) to dissolve the residue for gel chromatography. 7.2 Purification 7.2.1 Gel chromatography purification 7.2.1.1 Gel Chromatographic Purification Conditions A) Gel purification column. 400 mm x 25 mm (id); Filler. Bio-Beads, S-X3, 38 m ~ 75 m, or equivalent Need to do before the leaching curve). B) mobile phase. cyclohexane-ethyl acetate (1 1, volume ratio); C) Flow rate. 5.0 mL/min; D) Sample loop. 5 mL; E) Collection time. 20 min ~ 25 min. 7.2.1.2 Gel Chromatographic Purification Procedure The extract was transferred to a centrifuge tube and centrifuged at 4 000 r/min for 3 min. The supernatant was transferred to a vial of the gel permeation chromatograph , According to the conditions of 7.2.1.1 purification, the collection of water below 45 ℃ water bath concentrated to near dry, add 5 mL of methanol dissolved, add 5 mL Water mix well. 7.2.2 Propane sulfonyl silyl silica gel cation exchange column purification The propanesulfonylsilyl silica gel cation exchange column was mounted on a solid phase extraction apparatus, 5 mL of methanol was added, the effluent was discarded, Add 5 mL 0.1 mol/L hydrochloric acid solution, discard the effluent. Add 7.2.1 of the solution, add 10 mL of methanol - water (1 1, volume ), Discard the effluent, evacuate to dry, add 10 mL of ammonia - methanol (5 95, volume ratio), and collect 10 mL of the effluent. in 45 ℃ water bath concentrated under reduced pressure to near dry. Accurately add 0.5 mL of acetone to dissolve the residue and set the volume for GC-MS detection. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. DB-5ms quartz capillary column, 30 m × 0.25 mm (id) × 0.25 μm (film thickness), or equivalent. B) Column temperature. 50 ° C (1 min) 20 ° C/min 300 (10 min). C) Inlet temperature. 250 ° C. D) Interface temperature. 280 ° C. E) Carrier gas. helium, purity greater than or equal to 99.999%. Flow rate. 1.0 mL/min. F) Injection volume. 2 μL. G) Injection mode. pulse splitless injection, pulse pressure 25 psi, delay 0.75 min, 0.75 min after the valve. H) ion source. electron bombardment source (EI). I) Ionization energy. 70 eV. J) solvent delay time. 8 min. K) Detection method. Select the ion monitoring mode. L) Select the ion and relative abundance. see Table 1 Table 1 Select the ion and relative abundance Select the ion (M/z) 224 (quant.) 225 226 210 Relative abundance (%) 100 61.7 9.0 11.3 7.3.2 Quantitative determination According to the sample solution of azole ring amine content of the situation, selected peak area similar to the standard working solution. Standard working solution and sample solution in azole ring The amine response value should be within the linear range of the instrument detection. Standard working solution and sample volume and other volume interspersed injection detection. Under the above chromatographic conditions, The retention time of the cypermethrin is about 10.5 mim. The total ion chromatogram of the standard is shown in Figure A.1 in Appendix A. 7.3.3 Qualitative determination The standard solution and sample solution are subject to the conditions specified in 7.3.1, if the sample solution and the standard solution in the same retention time peak Now, it is confirmed by mass spectrometry, after deducting the background of the sample spectrum, the selected ions all appear, while the selected ion from the The abundance ratio is consistent with the relative abundance of the ions associated with the standard, and the fluctuation range is within the maximum allowable deviation of Table 2 (see Table 2) The presence of azoxycarbonylamine in the sample. The confirmed sample can be judged as azoxicillinamine positive detection. The spectrum of the cypermethrin standard is shown in the Appendix A in Figure A.2. Table 2 Mass Spectrometry Relative Ion Abundance Maximum Allowable Deviation 7.3.4 Blank test In addition to the sample, according to the above test steps. Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50%

8 results calculated

Use the chromatographic data processing software or the formula (1) to calculate the residual content of azoxicillin in the sample. A × c × V X = (1) AS x m Where. X - Residues of azoxicillin residues in milligrams per kilogram mg/kg; A - the peak area of azoxicillin in sample solution; C - the concentration of azoxicillin in the standard working fluid, in microns per milliliter g/mL; V - final volume of volume in milliliters of mL; AS - standard working area of azole ring amine peak area; M - the amount of sample represented by the final sample, in grams. 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 reproducible conditions and their arithmetic mean (percentage) shall be in accordance with the Record 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 the Record the requirements of D. 10% limit and recovery rate 10.1 Quantitation limits The limits of this method are 0.0004 mg/kg for honey and shrimp and 0.01 mg/kg for other samples. 10.2 Recovery rate The experimental data on the concentration, recovery and precision of the sample are given in Appendix B.

Appendix A

(Informative) Chromatograms and spectra Figure A.1 Total ion chromatogram of azoxicamines Figure A.2 Mass spectrum of azoxicicyclic amine reference substance

Appendix B

(Informative) Sample concentration and recovery of the experimental data Table B.1 Experimental data on the concentration and recovery of the sample Add concentration (Mg/kg) Recovery rate range% precision degree% Sample added concentration (Mg/kg) Recovery rate Precision% Rice 0.01 77.5 ~ 112 15.4 Tea 0.01 69.8 ~ 114 21.0 0.02 77.5 to 107 12.4 0.02 72.5 to 86.0 10.2 0.05 77.8 to 102 10.4 0.05 77.0 to 106 12.4 Sweet pea 0.01 78.2 ~ 113 13.9 Beef 0.01 78.9 ~ 113 14.7 0.02 77.5 to 110 13.4 0.02 78.8 to 103 10.6 0.05 79.6 ~ 104 10.0 0.05 83.0 ~ 102.2 10.6 Komatsu 0.01 75.1 ~ 102 11.5 Chicken 0.01 78.1 ~ 113 14.2 0.02 79.5 to 110 11.3 0.02 79.5 to 107 12.6 0.05 75.8 to 96.4 9.59 0.05 81.6 to 102 12.3 Pear 0.01 76.7 ~ 112 14.8 Shrimp 0.0004 56.5 ~ 85.5 15.9 0.02 79.5 ~ 107 11.7 0.0008 58.4 ~ 87.9 18.0 0.05 77.6 to 108 12.3 0.002 68.0 to 84.0 7.8 Citrus 0.01 69.1 ~ 112 18.0 Honey 0.0004 54.5 ~ 81.0 14.4 0.02 76.0 ~ 108 15.2 0.0008 56.8 ~ 82.9 14.4 0.05 80.2 to 110 13.2 0.002 62.5 to 81.5 10.8 Peanut 0.01 78.5 to 114 13.5 Soybean 0.01 73.8 to 107 16.4 0.02 79.5 to 111 13.2 0.02 75.0 to 104 12.0 0.05 79.4 to 108 14.0 0.05 79.6 to 110 13.5

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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