GB 23200.59-2016 English PDF

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GB 23200.59-2016: Food safety national standard -- Determination of residual glycosides in food by gas chromatography-mass spectrometry
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Basic data

Standard ID: GB 23200.59-2016 (GB23200.59-2016)
Description (Translated English): Food safety national standard -- Determination of residual glycosides in food by gas chromatography-mass spectrometry
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Word Count Estimation: 12,175
Date of Issue: 2016-12-18
Date of Implementation: 2017-06-18
Older Standard (superseded by this standard): SN/T 2385-2009
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 23200.59-2016: Food safety national standard -- Determination of residual glycosides in food by gas chromatography-mass spectrometry

---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Food safety national standard - Determination of residual glycosides in food by gas chromatography - mass spectrometry Instead of SN/T 2385-2009 ICS National Standards of People's Republic of China GB National standards for food safety Determination of residual glycosides in foodstuffs Gas chromatography - mass spectrometry National food safety standards- Determination of dichlobenil 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 2385-2009 "Determination of residual glycosides in imported and exported foods by gas chromatography-mass spectrometry". Compared with SN/T 2385-2009, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name 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 2385-2009. National standards for food safety Determination of residual glycosides in foodstuffs Gas chromatography - mass spectrometry

1 Scope

This standard specifies the method for the determination of diclofenac in food by gas chromatography-mass spectrometry. This standard applies to rice, soybeans, chestnuts, spinach, onions, mushrooms, tomatoes, mango, oranges, blackberries, watermelons, pork And milk in the amount of residual glycosides in the 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 file. 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 of the method

The residual dinoxazone was extracted with acetonitrile and purified by solid phase extraction (SPE) column. The gas chromatography-mass spectrometer 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 Acetonitrile (CH3CN). 4.1.2 Toluene (C7H8). 4.1.3 Acetone (C3H6O). 4.1.4 Diethylene glycol (C4H10O3). Analytical purity. 4.1.5 Sodium chloride (NaCl). Analytical purity. 4.1.6 anhydrous sodium sulfate (Na2SO4). analytical grade. Burned at 650 ℃ for 4 h, placed in the dryer in the spare. 4.2 solution preparation 4.2.1 Protective agent. 2% diethylene glycol-acetone solution. Take 100 mL of acetone, add 2 mL of diethylene glycol, mix well. 4.2.2 Eluent. acetonitrile - toluene (3 1, V/V). Take 150 mL of acetonitrile, add 50 mL of toluene, mix well. 4.3 standards 4.3.1 Dichlobenil. CAS No. 1194-65-6, Molecular formula. C7H3Cl12N, molecular weight 172.02, purity ≥99%. 4.4 standard solution preparation 4.4.1 Dichlorvoside standard stock solution. accurately weighed the amount of diclofenac standard (accurate to 0.1 mg), dissolved in toluene, prepared into 1000 μg/mL of standard stock solution, stored at -18 ° C. 4.4.2 Dichlorvoside standard working solution. dilute to the appropriate concentration of standard working solution with toluene as needed. 0.1 μg/mL standard work The solution was stored at -18 ° C. 4.5 Materials 4.5.1 Graphitized Carbon Solid Phase Extraction Column. ENVI-Carb, 6 mL, 500 mg, or equivalent. Add 1 ~ 2 g of anhydrous sulfur before use Sodium acetate, activated with 10 mL of acetonitrile-toluene. 4.5.2 C18 solid phase extraction column. C18,6 mL, 1000 mg, or equivalent. Add 1 ~ 2 g of anhydrous sodium sulfate before use, add 10 mL Acetonitrile - toluene activation. 4.5.3 Microporous membrane. 0.45μm, organic phase.

5 instruments and equipment

5.1 Gas Chromatography-Mass Spectrometer. Equipped with electron impact ionization source (EI). 5.2 Crusher. 5.3 Tissue crusher. 5.4 Balance. 0.01 g and 0.0001 g. 5.5 Ultrasonic Oscillator. 5.6 Centrifuge. speed greater than 4000r/min. 5.7 Vortex Mixer. 5.8 Automatic rapid concentrator (nitrogen blowing instrument). 5.9 Polytetrafluoroethylene centrifuge tube. 50mL, with plug.

6 Preparation and storage of samples

6.1 rice, soybeans, chestnuts 500 g of the sample was taken and pulverized with a pulverizer. Mix, are divided into two as a sample, into the clean Sheng Sheng bag, sealed Stored at 0 ~ 4 ℃. 6.2 mango, blackberry, watermelon, tomato, onion, spinach, oranges, mushrooms After picking the sample 1000 g, (without water washing), the sample was processed into a slurry by a mashing machine. Mix, are divided into Two as a sample, into the clean Sheng Sheng bag, sealed. The sample was stored at -18 ° C or lower. 6.3 pork Take 500 g of pork and chicken liver samples, and then chopped the samples into a slurry and mix them into two pieces. Sample, into the clean Sheng Sheng bag, sealed. The sample was stored at -18 ° C or lower. 6.4 milk Take about 500 g of the sample, mix, are divided into two as a sample, into the clean vial, sealed. Will sample on 0 ~ 4 ℃ under the conditions of preservation. Note. During the operation of the sample preparation, the sample should be prevented from being contaminated or the change in the residual content of the diclofenac. Note. The above sample sampling site according to GB 2763 Appendix A implementation.

7 Analysis steps

7.1 Extraction 7.1.1 Milk, pork, rice, soybeans Weigh 5 g (accurate to 0.01 g) sample in 50 mL polytetrafluoroethylene centrifuge tube, add 5 mL of water to mix and soak for 10 min. Join B Nitrile 10 mL, homogenized at 10000 r/min 0.5min, add 5 g sodium chloride, shake, ultrasonic extraction at 40 ℃ for 20min, at 8000 R/min centrifugal 8min, remove the upper organic phase with 2 ~ 3g anhydrous sodium sulfate funnel to the concentration of the bottle; then add 10 mL of acetonitrile, shake Uniform, ultrasonic extraction at 40 ℃ for 20min, 8,000 r/min centrifugation 8min, remove the upper organic phase with 2 ~ 3g anhydrous sodium sulfate Funnel to the concentrated flask, merge the extracted organic phases twice, then rinse the funnel with about 5 mL of acetonitrile and add 2 mL Curing agent, concentrated below 40 ℃ to about 1 mL, to be purified. 7.1.2 Mango, Blackberry, Watermelon, Oranges, Tomatoes Weigh 5 g (accurate to 0.01 g) sample in a 50 mL polytetrafluoroethylene centrifuge tube. Accurately add acetonitrile 10 mL, the following steps With 7.1.1. Concentrated below 40 ° C to about 1 mL, to be purified. 7.1.3 Onions, spinach, mushrooms, chestnuts Weigh 5 g (accurate to 0.01 g) sample in a 50 mL polytetrafluoroethylene centrifuge tube. Accurately add acetonitrile 10 mL, the following steps with the same 7.1.1. Concentrated below 40 ° C to about 1 mL, to be purified. 7.2 Purification 7.2.1 C18 solid phase extraction column purification The C18 solid phase extraction column was mounted on a vacuum suction apparatus of a solid phase extraction column, and the solution to be purified in the steps "7.1.1 and 7.1.3" Body column, after sample and then 2 mL eluent repeatedly washed and concentrated bottle, and then with 8 mL eluent for elution, the entire solid phase extraction purification The programmed flow rate does not exceed 6 mL/min. Consolidate the sample solution and eluent about 12 mL in the test tube, 40 ℃ below concentrated to near dry. With toluene Dissolved and fixed to 1.0 mL, and over 0.45 μm organic phase filter, gas chromatography - mass spectrometry. 7.2.2 Graphitized carbon solid phase extraction column purification A graphitized carbon solid phase extraction cartridge was mounted on a vacuum suction apparatus of a solid phase extraction column, and the solution to be purified in the step "7.1.2" Body column, after sample and then 2 mL eluent repeatedly washed and concentrated bottle, and then with 8 mL eluent for elution, the entire solid phase extraction purification The programmed flow rate does not exceed 6 mL/min. Collect the sample solution and eluent about 12 mL in the test tube, 40 ℃ below concentrated to near dry. With toluene Dissolved and fixed to 1.0mL, and over 0.45 μm organic phase filter, gas chromatography - mass spectrometry. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A column. DB-5 ms quartz elastic capillary column, 30 m × 0.25 mm (id), film thickness 0.25 μm, or equivalent By. B column temperature. 110 ℃ for 1min, 10 ℃/min heating to 160 ℃ for 2min, 20 ℃/min temperature to.200 ℃, the most After running at 300 ° C for 5 min. C Inlet temperature. 280 ° C. D Chromatography - Mass Spectrometer Interface Temperature. 280 ° C. E Carrier gas. helium, purity greater than or equal to 99.999%, flow 1.0 mL/min. F Injection volume. 2 μL. G Injection method. splitless injection, opening time. 1.5min. H ion source. EI. I ionization energy. 70 eV. J ion source temperature. 230 ° C. K quadrupole temperature. 150 ° C. L Data acquisition mode. Select the ion monitoring mode (SIM). M Select the ion (m/z). Quantitative ion. 171; Qualitative ion (abundance ratio). 173 (62.4), 136 (30.8), 100 (31.4) (Select only 173 and 136 as qualitative ions for onions and tomatoes). N solvent delay time. 5.8 min. 7.3.2 Quantitative determination According to the sample solution of the enemy in the case of nitrile, select the concentration of similar standard working solution. Standard working solution and solution of dextran The value should be within the linear range of the instrument detection. Standard working solution and sample volume and other volume interspersed injection determination. Under the above chromatographic conditions, The retention time of the oxalonitrile is about 6.0 min. 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 checked according to the above conditions, 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 The abundance of ions is consistent with the relative abundance of the ions associated with the standard, and the relative ion abundance deviation does not exceed the specified range of Table 1, In the presence of dioxin. The total ion flow chart and mass spectrum of the Energoxide standard are shown in Figures A.1 and A.2 in Appendix A. Table 1 qualitative determination of the relative ion abundance of the maximum allowable deviation 7.4 blank test In addition to no sample, according to the above steps.

8 results are calculated and expressed

The residual amount of dinitril in the sample can be calculated automatically by GC-MSD data processing software according to the external standard method and can be calculated according to formula (1) MAs VcA   (1) Where. X - the amount of residual glycosides in the sample, in micrograms per kilogram (μg/kg); The peak area (or peak height) of the enoxylate in the A - sample solution; The peak area (or peak height) of the quantitative ion chromatographic peaks of the dexamethasone in the standard working fluid; C - the concentration of dioxin in the standard working solution, in ng/ml for ng/ml; V - Final volume of volume in milliliters, mL; M - the mass of the 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 this method is 5 μg/kg. 10.2 Recovery rate The range of concentration and recovery of this method is given in Appendix B. Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50%

Appendix A

(Informative) Comparison of standard solution of Figure A.1 Selective ionization of standard solution GC-MS/EI for dinitriles Total ion chromatogram Figure A.2 Total Scanning Mass Spectrometry of GC-MS/EI

Appendix B

(Informative) Sample concentration and recovery of the experimental data Table B.1 Addition Concentration and Recovery Range of Dietoxan in Different Substrate Samples (%) (n = 6) Sample concentration (μg/kg) Recovery rate range (%) Rice 5 83.2 ~ 103.3 10 81.5 ~ 101.4 50 72.9 to 102.2 Soybeans 5 80.6 ~ 101.2 10 83.3 ~ 96.5 50 70.6 ~ 102.5 spinach 5 83.9 ~ 100.5 10 72.9 ~ 101.6 50 72.9 ~ 97.4 onion 5 64.1 to 94.4 10 71.6 ~ 95.8 50 71.1 to 102.1 Mushrooms 5 81.7 ~ 100.1 10 85.9 ~ 98.5 50 71.6 ~ 95.0 pork 5 82.2 ~ 96.2 10 75.7 to 103.9 50 72.3 ~ 92.3 milk 5 77.1 to 99.2 10 75.2 to 96.1 50 75.2 ~ 97.4 tomato 5 73.9 ~ 103.3 10 81.8 ~ 103.0 100 80.4 to 92.1 Mango 5 81.6 ~ 107.8 10 75.0 ~ 100.7 200 80.1 to 97.1 watermelon 5 72.4 ~ 96.3 10 70.5 to 108.3 200 80.8 ~ 92.2 orange 5 70.5 to 92.8 10 71.4 ~ 105.0 200 80.1 to 95.8 chestnut 5 84.6 ~ 103.6 10 72.6 ~ 104.7 200 81.2 ~ 96.2 blackberries 5 71.8 ~ 94.8 10 70.5 to 95.6 200 80.2 to 93.5

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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