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GB 23200.10-2016Food safety national standard -- Determination of 488 pesticides and related chemicals residues in mulberry, honeysuckle, medlar and lotus leaf by gas chromatography-mass spectrometry (English PDF)

桑枝、金银花、枸杞子和荷叶中488种农药及相关化学品残留量的测定气相色谱-质谱法

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Issued by

National Health and Family Planning Commission of the People 's Republic of China

Level / Type

National · Mandatory

Issue date

December 18, 2016

Implementation date

June 18, 2017

Scope

GB 23200.10-2016 is the English-translated version of 桑枝、金银花、枸杞子和荷叶中488种农药及相关化学品残留量的测定气相色谱-质谱法.

GB 23200.10-2016 — This standard specifies the residues of 488 pesticides and related chemicals (see Appendix A and Appendix F) residues of mulberry, honeysuckle, medlar and lotus leaf Quantitative Gas Chromatography - Mass Spectrometry.

This standard applies to the qualitative identification of 488 pesticides and related chemicals in mulberry, honeysuckle, medlar and lotus leaf, 431 pesticides and phase Quantitative determination of chemicals, other food can refer to the implementation.

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Document preview — GB 23200.10-2016

National Standard of the People's Republic of China

Classification: G 25
Replacing: GB/T 23200-2008

Issued by: National Health and Family Planning Commission of the People 's Republic of China

Preface
1 Scope
2 Normative reference document
Principle
4 Reagents and materials
5 Instruments and equipment
6 Preparation and storage of sample
7 Analysis Step
Calculation and presentation of results
9 Precision
10% limit and recovery rate
Appendix A (informative) 488 pesticides and related chemicals Chinese and English names, methods Quantitative limits, grouping, solvent selection

Foreword

This standard replaces GB/T 23200-2008 "residues of 488 pesticides and related chemicals in mulberry, honeysuckle, medlar and lotus leaf Determination of gas chromatography - mass spectrometry ".

This standard compared with GB/T 23200-2008, the main changes are as follows.

- Standard text format is modified to national standard text format for food safety;

- increase the "other food reference implementation" in the standard range.

This standard replaced the previous version of the standard release.

-GB/T 23200-2008.

National standards for food safety 818 kinds of pesticides and related chemical residues in mulberry, honeysuckle, medlar and lotus leaf Determination of gas chromatography - mass spectrometry

1 Scope

This standard specifies the residues of 488 pesticides and related chemicals (see Appendix A and Appendix F) residues of mulberry, honeysuckle, medlar and lotus leaf Quantitative Gas Chromatography - Mass Spectrometry.

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 samples were extracted with acetonitrile homogenate, salted out by centrifugation, solid phase extraction column, eluted with n-hexane-acetone and related chemicals.

Chromatography - mass spectrometry, internal 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 Acetonitrile (CH3CN, 75-05-8). Chromatographic Purification.

4.1.2 sodium chloride (NaCl, 7647-14-5). excellent grade pure.

4.1.3 dichloromethane (CH2Cl2, 75-09-2). chromatographic purity.

4.1.4 Acetone (CH3COCH3, 67-64-1). Chromatographic pure.

4.1.5 n-Hexane (C6H14,110-54-3). Chromatography pure, re-distillation.

4.1.6 Toluene C7H8, 108-88-3). Chromatographic Purification.

4.1.7 anhydrous sodium sulfate (Na2SO4,7757-82-6). analytical grade. 650 °C burning 4h, stored in a dryer, cooling and standby.

4.2 Standards

Pesticide and Related Chemical Reference Material. Purity >=95%, see Appendix A.

4.3 Standard solution preparation

4.3.1 Standard stock solution

Respectively, to take appropriate (accurate to 0.1mg) a variety of pesticides and related chemical standards were 10mL volumetric flask, according to the standard Solvents Toluene, toluene-acetone mixture, dichloromethane and other solvents (solvents are used chromatographic pure) dissolved and fixed to the scale (solvent Select the reference to Appendix A), the standard solution from light 0 °C ~ 4 °C preservation, shelf life of one year.

4.3.2 Mixing standard solutions (mixed standard solutions A, B, C, D, E and F)

According to the nature and retention time of pesticides and related chemicals, 488 kinds of pesticides and related chemicals are divided into A, B, C, D, E, F Six groups and determine their concentration in the mixed standard solution based on the response sensitivity of each pesticide and associated chemical on the instrument. This standard refer to Appendix A for the grouping of 488 pesticides and related chemicals and their mixed standard solution concentrations.

Depending on the group number of each pesticide and associated chemical, the concentration of the standard solution and the concentration of the standard stock solution, Pesticide and related chemicals standard stock solution in a 100mL volumetric flask, with toluene volume to the scale. Mixed standard solution light 0 °C ~ 4 °C Save, save for one month.

4.3.3 Internal standard solution

Accurately weigh 3.5 mg Epoxy Heptachlor in a 100 mL volumetric flask and settle with a volume of toluene.

4.3.4 Matrix mixed standard working solution

A, B, C, D, E, F group of pesticides and related chemical matrix mixed standard working solution is 40 µL internal standard solution and a certain volume the mixed standard solutions of A, B, C, D, E and F were added to 1.0 mL of the sample blank matrix extract respectively, Standard working solutions A, B, C, D, E and F. Matrix mixed standard working solution should be used with the current distribution.

4.4 Materials

4.4.1 Solid phase extraction column. CleanertTPH1) 10 mL, 2.0 g, or equivalent.

4.4.2 Microporous membrane (nylon). 13mm × 0.2µm.

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 Rotary Evaporator.

5.4 Homogenizer. The maximum speed is 24 000 r/min.

5.5 Centrifuge. Maximum speed is 4.200 r/min.

5.6 chicken heart bottle. 150 mL.

5.7 Pipettes. 1 mL.

6 Preparation and storage of samples

6.1 Preparation of the sample

Will be mulberry, honeysuckle, medlar and lotus leaf four kinds of Chinese herbal medicine grinding into fine powder, the sample all over 425µm standard mesh sieve, mix, the prepared samples are divided into two parts, packed in a clean container, sealed and marked.

7 Analysis steps

7.1 Extraction

Respectively, to take honeysuckle, medlar sample 5 g or lotus leaf, mulberry sample 2.5 g (accurate to 0.01g) in 50mL centrifuge tube, plus Into 15 mL of acetonitrile, (wolfberry fruit samples need to add 5 mL of water), 15000 r/min homogenate extraction 1min, add 2 g sodium chloride, and then homogenate Extract 1min, 4200 r/min centrifugal 5 min, take all the supernatant in 150mL chicken heart bottle, and then in the centrifuge tube by adding 15 mL of acetonitrile, Repeat the homogenate for 1 min, centrifuge at 4200 r/min for 5 min, take all the supernatant and the previous extract combined, the extract in 40 °C water Bath rotation to 1mL ~ 2 mL, to be purified.

7.2 Purification

Add about 2 cm high anhydrous sodium sulphate to the CleanertTPH solid phase extraction column and place it on a holder. Before loading, add 10mL Alkyl-acetone solution, the sample concentrate (7.1) is rapidly moved into the column when the pre-wash liquid level reaches the top of the anhydrous sodium sulfate, and receive the leaching solution with a chicken heart bottle. Wash the heart with 2 mL n-hexane-acetone solution, repeat three times, the same washing liquid into the column, the column was connected to a 25 mL reservoir and the pesticide and related chemicals were eluted with 25 mL of n-hexane-acetone solution. The eluent was rotated at 40 ° C Concentrated to near dry, add 1 mL of n-hexane dissolved residue, add 40 µL internal standard solution, mix, 0.2 µm filter, gas chromatography - Mass spectrometry.

7.3 Determination

7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions

A) Column. DB-1701 quartz capillary column [14% cyanopropyl-phenyl-methylpolysiloxane; 30 m x 0.25 mm (inner diameter), 0.25 Mm] or equivalent.

B) Column temperature. 40 °C for 1 min, then 30 °C/min program temperature to 130 °C, then 5 °C/min temperature to 250 °C, and then to 10 °C/min temperature to 300 °C, keep 5 min;

C) Carrier gas. helium, purity >=99.999%, flow rate. 1.2 mL/min;

D) Inlet temperature. 290 ° C;

E) Injection volume. 1 µL;

F) Injection method. no split injection, 1.5 min after the opening valve;

G) electron bombardment source. 70 eV;

H) ion source temperature. 230 ° C;

I) GC-MS interface temperature. 280 ° C;

J) solvent delay. 8.3 min in group A, 7.8 min in group B, 7.3 min in group C, 5.5 min in group D, 6.1 min in group E, 6.1 min in group E, Group was 5.5 min;

Cleanert TPH is a trade name of Agela's products, and this information is intended for the convenience of users of this standard and is not intended to endorse the product. If other equivalent Products have the same effect, you can use these equivalent products.

K) Select the ion monitoring. each compound selected a quantitative ion, 2 ~ 3 qualitative ions. Each group needs to be tested Ions in accordance with the peak sequence, respectively, sub-time detection. The retention time of each compound, the quantitative ion, the qualitative ion and the quantitative ion for the abundance ratio of qualitative ions, see Appendix B. Refer to Appendix C for the start time and residence time of each group to detect ions.

7.3.2 Qualitative determination

When the sample is measured, if the retention time of the detected peaks is consistent with the standard sample, and after the background mass in the figure, the selected ions are present, and the selected ion abundance ratio is consistent with the ion abundance ratio of the standard sample (relative abundance > 50% Allow ± 10% deviation; relative abundance > 20% to 50% allow ± 15% deviation; relative abundance > 10% to 20% allow ± 20% deviation;

Relative abundance <= 10%, allowing ± 50% deviation), you can determine the presence of this pesticide or related chemicals in the sample. If it can not be confirmed, should be heavy New injection, in scanning mode (with sufficient sensitivity) or by adding other confirmed ions or with other higher sensitivity analytical instruments to confirm.

7.3.3 Quantitative determination

This standard uses the internal standard method of single ion quantitative determination. The internal standard is epoxy heptachlor. To reduce the impact of the matrix, quantitative standards should be used Quality sample solution mixed with standard working solution. The concentration of the standard solution should be close to the concentration of the compound to be tested. The method of A, B, C, D, E, F group of reference substances in the wolfberry matrix selection of ion monitoring GC-MS Figure see Appendix D.

7.4 Parallel test

Perform the parallel test of the same sample according to the above steps.

7.5 Blank test

Unless the sample is not weighed, according to the above steps.

8 Results are calculated and expressed

The result of gas chromatography-mass spectrometry can be calculated automatically by computer according to internal standard method, and can be calculated according to formula (1) Xi = cs × Ci Asi (1) as csi Ai m 1000 where.

Xi - Residue of the test substance in milligrams per kilogram (mg/kg);

Cs - the concentration of the test substance in the standard working solution in micrograms per milliliter (µg/mL);

A - the chromatographic peak area of the analyte in the sample solution;

As - the chromatographic peak area of the test substance in the matrix standard working solution;

Ci - the concentration of the internal standard in the sample solution, in micrograms per milliliter (µg/mL);

Csi - the concentration of the internal standard in the standard working solution of the matrix, in micrograms per milliliter (µg/mL);

Asµ - the chromatographic peak area of the internal standard in the matrix standard working solution;

Ai - the chromatographic peak area of the internal standard in the sample solution;

V - the final volume of the sample solution in milliliters (mL);

M - the mass of the sample represented by the sample solution, in grams (g).

The result of the calculation should be deducted from the blank value. The result of the measurement is expressed by the arithmetic mean of the parallel measurement, and the two valid digits are 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 the requirements of E.

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 F requirements.

10% limit and recovery rate

10.1 Quantitation limits

The quantitative limits of this method are given in Appendix A.

10.2 Recovery rate

When adding levels of LOQ, 20 × LOQ, add the recovery rate see Appendix G.

Appendix A

(Informative)

488 kinds of pesticides and related chemicals Chinese and English name, method of quantitative limit, grouping, solvent selection and mixed standard solution concentration A.1 488 Pesticides and Related Chemicals Chinese and English Name, Method Quantification Limits, Grouping, Solvent Selection and Mixing Standard Solution Concentration See Table A.1

Table A.1

unit.%

Serial number Chinese name English name the limit of quantitation/Solvent Mixed standard Solution concentration / (Mg/L) (Mg/kg) Internal standard epoxy heptachlor-epox Group A 1 2-Propyl Acetate allidochlor 0.0500 Toluene 5 2 allyl chloride dichlormid 0.0500 toluene 5 3 soil fungus etridiazol 0.0750 toluene 7.5

4 Chloromethylthiophosphate chlormephos 0.0500 Toluene 5 5 aniline spirit propham 0.0250 toluene 2.5 6 ring grass enemy cycloate 0.0250 toluene 2.5 7 biphenyl diamine diphenylamine 0.0250 toluene 2.5 8 chlordimeform chrysanthemum 0.0250 n-hexane 2.5

9 Ethylene Bromine Ethalfluralin 0.1000 Toluene 10 10 phorate 0.0250 toluene 2.5 11 methyl ethyl phthalide thiometon 0.0250 toluene 2.5

12 Pentachloronitrobenzene quintozene 0.0500 Toluene 5

13 Deethyletrazine atrazine-desethyl 0.0250

Toluene Acetone

14 isosubicin clomazone 0.0250 toluene 2.5 15 diazinon 0.0250 toluene 2.5 16 toxaphene fonofos 0.0250 toluene 2.5 17 spiramide etrimfos 0.0250 toluene 2.5

18 Amipropion propetamphos 0.0250 Toluene 2.5

19 Sec. Sec. Secancourt

20 Propargyl grass amine pronamide 0.0250

Toluene Acetone

21 Removal of phosphorus dichlofenthion 0.0250 Toluene 2.5 22 zwick mexacarbate 0.0750 toluene 7.5 23 dimethoate 0.1000 toluene 10

24 Amificin dinitramine 0.1000 Toluene 10 25 aldrin 0.0500 toluene 5 26 dolphin phosphorus ronnel 0.0500 toluene 5 27 promised net prometryne 0.0250 toluene 2.5

28 Cycloprozine cyprazine 0.0250

Toluene Acetone

29 Vermoderma vellozolin 0.0250 Toluene 2.5

30? -hexachlorazine-HCH 0.0250 Toluene 2.5 31 metalaxyl 0.0750 toluene 7.5 32 methyl parathion 0.1000 Toluene 10 Serial number Chinese name English name the limit of quantitation/Solvent Mixed standard Solution concentration / (Mg/L) (Mg/kg)

33 Chlorpyrifos (-ethyl) 0.0250 toluene 2.5

34 delta-six six six delta-HCH 0.0500 Toluene 5 35 times thiophosphate fenthion 0.0250 toluene 2.5 36 malathion 0.1000 Toluene 10 37 paraoxon-ethyl 0.8000 toluene 80 38 fenitrothion 39 triazolone triadimefon 0.0500 toluene 5

40 Lee Valley Long linuron 0.1000

Toluene Acetone

41 pendimethalin 0.1000 toluene 10

42 Acylidene chloride

43 Ethyl bromothiophosphate bromophos-ethyl 0.0250 Toluene 2.5 44 quetiapine quinalphos 0.0250 toluene 2.5

45 Trans-chlordane 0.0250 toluene 2.5

Potato powder scattered phenthoate 47 pyrazolamine metazachlor 0.0750 toluene 7.5 48 propithiol prothiophos 0.0250 toluene 2.5 49 shaped plastic chlorfurenol 0.0750 Toluene Acetone (9 1) 7.5

50 Pythium Bermidipine 0.0250 Toluene 2.5

Dieldrin 0.0500 Toluene 5

52 Methamidone A methidathion 0.0500 Toluene 5

53 Dihydroxylamine napropamide 0.0750 Toluene 7.5

54 Cyanocobalt cyanazine 0.0750

Toluene Acetone

55 maloxine oxadiazone 0.0250 toluene 2.5 56 benzene line phosphorus fenamiphos 0.0750 toluene 7.5 57 acaricides sulfur sulfide tetrasul 0.0250 toluene 2.5

58 Ethyl pyrimethanol sulfonate bupirimate 0.0250 Toluene 2.5 59 fluoroamide a flutolanil 0.0250 toluene 2.5

60 Moisturizer a carboxin 0.6000 Toluene 60 61 p, p'-drop p, p'-DDD 0.0250 toluene 2.5

62 Ethiophenazine Ethion 0.0500 Toluene 5

63 Acetazole-1 etaconazole-1 0.0750 Toluene 7.5 64 thiophosphate sulprofos 0.0500 toluene 5 65 etetonazole-2 etaconazole-2 0.0750 toluene 7.5 66 myclobutamycin myclobutanil 0.0250 toluene 2.5

67 Forskophil Pineulfothion 0.0500 Toluene 5

68 grass spirit diclofop-methyl 0.0250 toluene 2.5 69 propiconazole-1 0.0750 toluene 7.5 70 propiconazole-2 0.0750 Toluene 7.5 71 bifenthrin 0.0250 n-hexane 2.5

72 Mirex mirex 0.0250 Toluene 2.5

73 Butylcyclopedia carbosulfan 0.0750 Toluene 7.5

Serial number Chinese name English name the limit of quantitation/Solvent Mixed standard Solution concentration / (Mg/L) (Mg/kg)

74 Fluorophenylpyrimidine nuarimol 0.0500

Toluene Acetone

75 wheat rust Ling benodanil 0.0750 Toluene 7.5

76 Oxygen DDT methoxychlor 0.2000 Toluene 20

77 Oxalic acid oxadixyl 0.0250 Toluene 2.5 78 tebuconazole 0.0750 toluene 7.5

79 Tetramethrin tetramethirn 0.0500 Toluene 5

80 Fluorfenin norflurazon 0.0250

Toluene Acetone

81 pyridazine sulfur phosphorus pyridaphenthion 0.0250 toluene 2.5

82 Dicofloxacin tetradifon 0.0250 Toluene 2.5 83 cis-permethrin 0.0250 toluene 2.5

84 Pyridobacillus pyrazophos 0.0500 Toluene 5 85 trans-permethrin 0.0250 toluene 2.5 86 cypermethrin 0.0750 toluene 7.5 87 fenvalerate-1 0.1000 Toluene 10 88 fenvalerate -2a fenvalerate-2 0.1000 Toluene 10

89 Deltamethrin 0.1500 toluene 15

Group B

90 Green grass enemy EPTC 0.0750 Toluene 7.5

Alkaline butylate 0.0750 Toluene 7.5

92 Diclovir dichlobenil 0.0050 Toluene 0.5 93 grams of grass enemy pebulate 0.0750 toluene 7.5

94 Trichloromethylpyridine nitrapyrin 0.0750 Toluene 7.5

95 Times the speed of phosphorus mevinphos 0.0500 toluene 5

Chlorobenzene Chloroneb 0.0250 Toluene 2.5 97 tetrachloronitrobenzene tecnazene 0.0500 toluene 5 98 heptenol heptanophos 0.0750 toluene 7.5 99 off line phosphorus ethoprophos 0.0750 toluene 7.5 100 hexachlorobenzene a hexachlorlorobenzene 0.0250 toluene 2.5 Glutanamine propachlor 0.0750 Toluene 7.5 102 cis - oat enemy cis-diallate 0.0500 toluene 5 103 trifluralin 0.0500 toluene 5 104 trans-diallate 0.0500 toluene 5

105 Chlorohydrin Ling chlorpropham 0.0500 Toluene 5

106 Cobalt Phosphotophor 0.0250 Toluene 2.5 107 cabbage malocide sulfallate 0.0500 toluene 5 108 alpha-hexahydrate alpha-HCH 0.0250 Toluene 2.5

109 Tbn thiophos terbufos 0.0500 Toluene 5

110 Ciprofloxacin profluralin 0.1000 Toluene 10 111 xanthoxine a dioxathion 0.1000 Toluene 10

112 Fighting Chin propazine 0.0250 Toluene 2.5

113 Chlorohydrin chlorbufam 0.0500 Toluene 5 Serial number Chinese name English name the limit of quantitation/Solvent Mixed standard Solution concentration / (Mg/L) (Mg/kg)

114 Chloronitamine dicloran 0.0500 Toluene 5 115 terbutaline terbuthylazine 0.0250 toluene 2.5

116 Green Valley Long monolinuron 0.1000 Toluene 10

117 Fluorfins flufenoxuron 0.0750 Toluene 7.5 118 methyl chlorpyrifos-methyl 0.0250 toluene 2.5 119 deer net desmetryn 0.0250 toluene 2.5 120 dimethachlor 0.0750 toluene 7.5 121 alachlor 0.0750 toluene 7.5

122 Methylpyrimidine Phosphorus pirimiphos-methyl 0.0250 Toluene 2.5 123 terbutinedine terbutryn 0.0500 toluene 5

124 Propionate aspon 0.0500 Toluene 5 125 kill the grass thiobencarb 0.0500 toluene 5 126 dicofol 0.0500 toluene 5 127 metolachlor 0.0250 toluene 2.5 Piperidine Phosphine pirimiphos-ethyl 129 benzofluorosulfonamide a dichlofluanid 1.2000 Toluene Acetone (9 1) 130 methoprene 0.1000 Toluene 10 131 bromothiophosphoric bromofos 0.0500 Toluene 5 132 ethofume orange 5 133 isopropylleol isopropalin 0.0500 toluene 5 134 propanil 0.0500 toluene 5 135 animal phosphorus crufomat...

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Referenced standards

Cited by

GB 2763-2026National food safety standard-Maximum residue limits for pesticides in food

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