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GB 23200.86-2016 English PDF

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GB 23200.86-2016: Food safety national standard -- Determination of residues of organochlorine pesticides in milk and dairy products by gas chromatography-mass spectrometry / mass spectrometry
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GB 23200.86-2016English279 Add to Cart 3 days [Need to translate] Food safety national standard -- Determination of residues of organochlorine pesticides in milk and dairy products by gas chromatography-mass spectrometry / mass spectrometry Valid GB 23200.86-2016

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Basic data

Standard ID GB 23200.86-2016 (GB23200.86-2016)
Description (Translated English) Food safety national standard -- Determination of residues of organochlorine pesticides in milk and dairy products by gas chromatography-mass spectrometry / mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 14,155
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 3036-2011
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 23200.86-2016: Food safety national standard -- Determination of residues of organochlorine pesticides in milk and dairy products by gas chromatography-mass spectrometry / mass spectrometry



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Food safety national standard - Determination of residues of organochlorine pesticides in milk and dairy products by gas chromatography-mass spectrometry/mass spectrometry IICSICSCS National Standards of People's Republic of China GB Instead of SN/T 3036-2011 National standards for food safety Determination of Residues of Organochlorine Pesticides in Milk and Dairy Products Gas chromatography - mass spectrometry/mass spectrometry National food safety standards- Determination of multiple residue of organochlorine pesticides in milk and dairy Products Gas chromatography - mass spectrometry 2016-12-18 Release.2017-06-18 Implementation People 's Republic of China Health and Family Planning Commission Ministry of Agriculture of the People 's Republic of China State Administration of Food and Drug Administration release

Foreword

This standard replaces SN/T 3036-2011 "Determination of residues of organochlorine pesticides in export milk and dairy products Gas chromatography-mass spectrometry / Mass spectrometry ". Compared with SN/T 3036-2011, 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 "export milk and dairy products" to "milk and dairy products"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 3036-2011. National standards for food safety Determination of Residues of Organochlorine Pesticides in Milk and Dairy Products Gas chromatography - mass spectrometry/mass spectrometry

1 Scope

This standard specifies methods for the determination of multiple organochlorine pesticide residues in milk and dairy products by gas chromatography-mass spectrometry/mass spectrometry. This standard applies to liquid milk, milk powder, yogurt (semi-solid), ice cream, milk and other milk and dairy products in a six six six, P, p'-DDT, o, p'-droplet, p, p'-droplet, o , P, p'-drop, Methotrexate, heptachlor, epoxidized heptachlor, aldrin, dieldrin, endrin, aldrin aldehydes, Trans-chlordane, chlorinated chlordane, α-endosulfan, β-endosulfan, endosulfan sulfate, hexachlorobenzene, tetrachloronitrobenzene, pentachloronitrobenzene, pentachloroaniline, Methyl pentachlorophenyl sulfide, mirex and other 30 kinds of organochlorine pesticide residues in the determination 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 organochlorine pesticide residue in the sample was extracted with n-hexane-acetone (1 1, volume ratio) solution, and the extract was concentrated and gel permeated Chromatography and Florian silica column were determined by gas chromatography - mass spectrometry/mass spectrometry and quantified by external standard area method.

4 reagents and materials

Unless otherwise specified, the reagents used are analytical grade and water is 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 dichloromethane (C2H2Cl2). chromatographic purity. 4.1.4 Cyclohexane (C6H12). 4.1.5 Ethyl acetate (C4H8O2). 4.1.6 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4 h, in the dryer to cool to room temperature, stored in a sealed bottle in reserve. 4.1.7 Sodium chloride (NaCl). 4.2 solution preparation 4.2.1 Extract. Take appropriate n-hexane and acetone in a 1. 1 by volume ratio. 4.2.2 Gel permeation chromatography Eluent. Take appropriate amount of cyclohexane and ethyl acetate in a 1. 1 by volume ratio. 4.2.3 Solid Phase Extraction Eluent. Take appropriate n-hexane and dichloromethane in a volume ratio of 5.95. 4.3 standards 4.3.1 Pesticide Reference Material. Purity ≥95%. 4.4 standard solution preparation 4.4.1 standard stock solution. accurately weighed the right amount of the standard material, with n-hexane prepared into a concentration of 100 μg/mL standard stock solution, The solution was stored at 0 ° C to 4 ° C in the dark. 4.4.2 standard intermediate solution. take appropriate amount of standard stock solution, prepared into a 2 μg/mL mixed standard working solution, the solution in the 0 ℃ ~ 4 ℃ dark preservation. 4.4.3 standard working solution. take appropriate amount of various standard stock solution, prepared into the appropriate concentration of mixed standard working solution. Standard work Liquid is now available. 4.5 Materials 4.5.1 Florisil Solid Phase Extraction Column. 1 g/6 mL, or equivalent, activated with 5 mL n-hexane prior to use. 4.5.2 Microporous membrane. 0.45 μm, organic.

5 instruments and equipment

5.1 Gas Chromatography - Mass Spectrometry/Mass Spectrometer. Electronically Bombardive Source (EI). 5.2 Gel Permeation Chromatography. 5.3 Electronic balance. 0.01 g and 0.0001 g. 5.4 Vortex Mixer. 5.5 Centrifuge. Maximum speed up to 5 000 r/min. 5.6 Rotary Evaporator. 5.7 nitrogen blowing instrument. 5.8 Centrifugal tube. Teflon, 50 mL.

6 Preparation and storage of samples

Liquid milk, yogurt, ice cream. take a representative of about 100 g, into a clean container as a sample, sealed and do the logo, at 0 ~ 4 ℃ Save the refrigerator. Milk powder, candy. take representative of about 100 g, into a clean container as a sample, sealed and do a good job, at room temperature Save During the sample preparation operation, it is necessary to prevent contamination of the sample or change in the content of the residue. Note. The above sample sampling site according to GB 2763 Appendix A implementation.

7 Analysis steps

7.1 Extraction Accurately weigh 10 g of sample (accurate to 0.01 g) in a 50 mL stoppered centrifuge tube (milk powder, lactose plus 10 mL of water), add 5 g of sodium chloride, add 10 mL of the extract, shake with a vortex mixer for 1 min, 4 000 r/min for 3 min, transfer the organic phase to 100 mL of rotary vials, the residue was extracted twice with 10 mL of the extract, the organic phase was centrifuged and concentrated by rotary evaporation at 40 ° C Close to dry, with 10 mL cyclohexane - ethyl acetate mixed solution to fully dissolve the residue, over 0.45 μm filter, to be purified. 7.2 Purification 7.2.1 Purification by gel permeation chromatography 7.2.1.1 Reference conditions A) Purification column. 400 mm × 25 mm (id), containing Bio-Beads, S-X3, 38 μm ~ 75 μm filler, or equivalent performance. B) mobile phase. cyclohexane-ethyl acetate (1 1, volume ratio); C) Flow rate. 5 mL/min; D) Injection volume. 5 mL; E) Start collection time. 10 min; F) End of collection time. 22 min. 7.2.1.2 Purification steps The solution to be purified was transferred to a 10 mL test tube and purged with a gel permeation chromatograph. The eluent was collected for 10 min to 22 min at 40 ° C And then concentrated to about 2 mL under reduced pressure to be purified by Fryborough silica solid phase extraction column. 7.2.2 solid phase extraction purification The sample was transferred to an activated florisil silica solid phase extraction column and the effluent was collected and washed with 8 mL of dichloromethane-n-hexane solution The eluate was collected by rotary evaporation at 40 ° C and concentrated to near dryness. The residue was dissolved in 1 mL of n-hexane and passed through a 0.45 μm filter for assay. The 7.3 Determination 7.3.1 Instrument reference conditions A) Column. TR-35 ms, 30 m × 0.25 mm × 0.25 μm, or equivalent; B) Column temperature. 55 ℃ for 1 min, at 40 ℃/min rate rose to 140 ℃, keep 5 min, at 2 ℃/min rate rose to 210 ℃, to 10 ℃/min rate rose to 280 ℃, keep 10 min; C) Inlet temperature. 250 ° C; D) ion source temperature. 250 ° C; E) Transmission line temperature. 250 ° C; F) ion source. electron bombardment ion source; G) Measurement method. Select the reaction monitoring mode (SRM); H) Monitoring ions (m/z). Qualitative ion pairs, quantitative ion pairs, collision energy and ion abundance of various organochlorine pesticides are given in Appendix A In Table A.1; I) Carrier gas. helium, purity not less than 99.999%; J) Flow rate. 1.2 mL/min; K) Injection method. no shunt; L) Injection volume. 1 μL; M) Ionization energy. 70 eV; 7.3.2 Determination and confirmation of chromatography Determination of sample solution and standard working solution according to 7.3.1 gas chromatography-mass spectrometry/mass spectrometry conditions, determination of organochlorine pesticide residues in sample solution by external standard method the amount. Residues to be measured in the sample should be within the standard curve, and if the residue exceeds the standard curve range, appropriate dilution should be made. in The retention times of the various organic chlorine mass chromatographic peaks under the above chromatographic conditions are given in Table A.1 in Appendix A. The total ion chromatogram of the standard and the multiple The chromatogram should be shown in Figure B.1 and Figure B.2 in Appendix B. Under the same experimental conditions, the relative retention time of the sample and the mass chromatographic peak of the test substance in the standard working fluid was within ± 2.5% And in the sample quality chromatogram after subtracting the background, the selected ion pair appears, and the relative abundance of the standard is not allowed The range specified in Table 1, you can determine the existence of the corresponding sample in the sample. Table 1 Gas Chromatography - Tandem Mass Spectrometry Qualification Relative Relative Absorption Error of Ion Abundance Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50% 7.4 blank test In addition to weighing the sample, according to the above steps.

8 results are calculated and expressed

The amount of organochlorine pesticide in the sample was calculated according to formula (1) using the external standard method in the data processing software or drawing the standard curve.  Vc X ii (1) Where. Xi - the amount of pesticide residues in the sample, in micrograms per kilogram (μg/kg); Ci - Concentration of the i component pesticide in the sample obtained from the standard curve, in micrograms per liter (μg/L); V - the final volume of the sample solution 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 B 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 C requirements. 10% limit and recovery rate 10.1 Quantitation limits The limit of quantification of various organochlorine pesticides in this method was 0.8 μg/kg. 10.2 Recovery rate The average recoveries of the method were 62.2% ~ 116.8%.

Appendix A

(Informative) Reference mass spectrometry conditions 1 Mass spectrometry conditions. A) Method mode. EZ method B) ion box. CEI (Close EI) C) ion source temperature. 250 ° C D) filament current. 25 μA E) Q1 peak width. 0.7 FWHM F) Cycle time. 0.5 s G) chromatographic filter peak width. 3.0 s H) collision gas. argon, the purity of not less than 99.999% I) Collision gas pressure. 1.5 mTorr J) Qualitative ion pair, quantitative ion pair, collision energy and ion abundance ratio are shown in Table A.1. Table A.1 Retention Time of 30 Organochlorine Pesticides, CAS, Qualitative Ion Pair, Quantitative Ion Pair and Collision Energy Time window (Min) Compounds keep time (Min) CAS parent ion (m/z) Ion (M/z) Collision energy (EV) Qualitative/quantitative ion Abundance ratio (%) 13.0 to 25.0 Tetrachloronitrobenzene 15.9 117-18-0 259.201 15 261 203 * 15 Hexachlorobenzene 19.6 608-73-1 286 251 * 20 Α 666 20.5 319-84-6 181 145 * 15 Pentachloronitrobenzene 23.2 82-68-8 295 237 * 20 Lindane 24.0 58-89-9 181 145 * 15 25.0 to 33.0 BHC 6 26.3 319-85-7 181 145 * 15 Heptachlor 27.1 76-44-8 272 237 * 15 Pentachloroaniline 27.8 527-20-8 265 158 * 30 Δ-six six six 28.8 319-86-8 181 145 * 15 Aldrin 29.9 309-00-2 263 193 * 32 Methyl pentachlorophenyl sulfide 31.3 1825-19-0 296 263 * 20 61 Table A.1 Retention Time, CAS, Qualitative Ion Pair, Quantitative Ion Pair and Collision Energy of 30 Organochlorine Pesticides (Continued) 1 Non-commercial declaration. The reference mass spectrometry conditions listed in Appendix A are performed on a thermo TSQ Quantum GC GC-Tandem Mass Spectrometer, listed here The test instrument model is for reference only and does not involve commercial purposes and encourages standard users to try different manufacturers or models of instruments. Oxidized Chlordane 34.1 27304-13-8 387 263 * 15 74 Epoxy heptachlor 35.2 28044-83-9 353 253 * 15 58 Trans-chlordane 37.2 5103-74-2 373 266 * 18 Cis-chlordane 38.3 5103-71-9 373 266 * 18 O, p'-drop i 38.4 72-55-9 246 176 * 25 Α-endosulfan 38.4 959-98-8 241 206 * 20 39.5 to 45.3 P, p'-droplet 40.5 72-55-9 246 176 * 25 Dieldrin 40.5 60-57-1 263 193 * 26 O, p'-drop 41.1 53-19-0 235 165 * 20 Endrin 41.9 72-20-8 263 193 * 26 O, p'-DDT 42.6 789-02-6 235 165 * 20 P, p'-drop 43.0 72-54-8 235 165 * 20 Β-endosulfan 43.0 33213-65-9 241 206 * 20 P, p'-DDT 43.9 789-02-6 235 165 * 20 Aldin Aldehydes 43.9 7421-93-4 345 317 * 10 Endosulfan sulfate 44.5 1031-07-8 272 237 * 15 45.3 ~ 48.0 Methanol DDT 46.1 72-43-5 227 169 * 20 Endrin Ketone 46.2 53494-70-5 317 281 * 10 Mirex 46.6 2385-85-5 272 237 * 15 Note. "*" Quantitative ions.

Appendix A

(Informative) Chromatogram RT. 0.00 - 47.31 0 5 10 15 20 25 30 35 40 45 Time (min) La Ti 41.45 42.65 43.00 43.95 46.63 38.36 46.15 27.14 37.15 19.55 31.32 29.9015.94 24.0723.26 35.1816.07 23.19 34.15 NL. 1.75E4 TIC MS 091024- 4ppb-2 Figure B.1 Total ion chromatogram of 30 organochlorine pesticide standard solutions (4 μg/L) Tetrachloronitrobenzene RT. 10.27 - 20.13 Time (min) La Ti E RT. 15.90 RT. 15.91 Hexachlorobenzene RT. 16.33 - 22.08 Time (min) La Ti E RT. 19.57 RT. 19.56 Six six six (α/ν/β/δ) RT. 18.47 - 30.44 Time (min) La Ti E RT. 28.75 RT. 26.27 RT. 24.05 RT. 28.76 RT. 26.29 RT. 20.54 RT. 20.32 - 28.81 Time (min) La Ti E RT. 23.22 RT. 23.24 Pentachloronitrobenzene heptachlor RT. 22.01 - 31.74 Time (min) La Ti E RT. 27.11 RT. 27.12 Pentachloroaniline RT. 23.35 - 32.66 24 26 28 30 32 Time (min) La Ti E RT. 27.75 RT. 27.72 Aldrin RT. 25.81 - 33.85 Time (min) La Ti E RT. 29.90 RT. 29.90 Pentachlorophenyl sulfide RT. 25.81 - 33.85 Time (min) La Ti E RT. 31.27 RT. 31.26 Oxidized Chlordane RT. 30.18 - 38.92 Time (min) La Ti E RT. 34.15 RT. 34.10 Epichlorohydrin RT. 30.18 - 38.92 Time (min) La Ti E RT. 35.20 RT. 35.18 Chlordane (trans/cis) RT. 34.51 - 40.43 Time (min) La Ti E RT. 37.15 RT. 38.30 RT. 37.16 RT. 38.27 DDE (op/pp) RT. 36.47 - 41.70 37 38 39 40 41 Time (min) La Ti E RT. 40.50RT. 38.36 RT. 38.93 RT. 40.48 RT. 38.36 RT. 38.66 Figure B.2 Selection of 30 Organochlorine Pesticide Standard Solutions Response Monitoring (SRM) Ion Chromatography Endosulfan (α/β) RT. 33.69 - 46.04 Time (min) La Ti E RT. 43.01 RT. 38.45 RT. 38.43 RT. 43.00 Dieldrin RT. 38.32 - 41.74 Time (min) La Ti E RT. 40.54 RT. 40.54 O, p '(DDD, DDT, p), p (DDD DDT) RT. 40.26 - 44.90 Time (min) La Ti E RT. 43.93RT. 42.63 RT. 42.98 RT. 41.43 RT. 43.93 RT. 42.63 RT. 42.98 RT. 41.43 Endrin RT. 40.80 - 45.70 41 42 43 44 45 Time (min) La Ti E RT. 41.96 RT. 41.94 Aldin aldehydes RT. 40.80 - 45.70 41 42 43 44 45 Time (min) La Ti E RT. 43.89 RT. 43.90 RT. 44.10 Endosulfan sulfate RT. 40.87 - 46.30 41 42 43 44 45 46 Time (min) La Ti E RT. 44.51 RT. 43.01 RT. 46.24 RT. 44.49 Methanol DDT RT. 40.30 - 47.31 Time (min) La Ti E RT. 46.12 RT. 46.12 Vitamin ketone RT. 44.31 - 47.30 Time (min) La Ti E RT. 46.24 RT. 46.64 RT. 46.24 Mirex RT. 44.31 - 47.30 Time (min) La Ti E RT. 46.63 RT. 46.64 RT. 44.51 RT. 46.24RT. 44.68

Appendix B

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

Appendix C

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

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