GB 23200.14-2016Food safety national standard -- Determination of 512 pesticides and related chemical residues in fruit and vegetable juices and fruit wine by liquid chromatography-mass spectrometry (English PDF)

Foreword

The standard instead of GB/T 23206-2008 "fruit and vegetable juice, fruit wine in the determination of 512 kinds of pesticides and related chemical residues liquid chromatography -Tandem mass spectrometry ".

This standard compared with GB/T 23206-2008, the main changes are as follows.

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

- the standard range to increase the "other fruit and vegetable juice, wine can refer to the implementation." this standard replaced the previous version of the standard release.

-GB/T 23206-2008.

National standards for food safety Determination of 512 pesticides and related chemical residues in fruit and vegetable juices and Liquid chromatography - mass spectrometry

1 Scope

This standard provides orange juice, apple juice, grape juice, cabbage juice, carrot juice, dried wine, semi-dry wine, semi-liqueur, liqueur 512 Pesticide and related chemicals (see Appendix A) Residue Liquid Chromatography - Mass Spectrometry.

This standard applies to orange juice, apple juice, grape juice, cabbage juice, carrot juice, dried wine, semi-dry wine, semi-liqueur, Pesticide and related chemical residues in the qualitative identification, but also for 490 kinds of pesticides and related chemical residues in the quantitative determination of other fruits and vegetables Juice, wine 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 sample was extracted with 1% acetonitrile solution, purified by Sep-Pak Vac column, eluted with acetonitrile-toluene solution (3 1) and related the samples were analyzed by liquid chromatography - tandem mass spectrometry and quantified by 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.

5 Instruments and equipment

5.1 Liquid Chromatography - Tandem Mass Spectrometer. Equipped with electrospray ion source.

5.2 Analysis of balance. 0.1 mg and 0.01 g.

5.3 chicken heart bottle..200 mL.

5.4 Pipettes. 1 mL.

5.5 Vials. 2 mL, with Teflon Capping.

5.6 with a plug centrifuge tube. 50 mL.

5.7 Scroll Mixer.

5.8 Nitrogen Drying Machine.

5.9 Low speed centrifuge. 4200 r/min.

5.10 Rotary Evaporator.

6 Sample preparation

Concentrate fruit and vegetable juice samples, all the original samples will be made into a clean enamel mixed barrels, stir well and mix well, then mix the goods are packed in two copies (500 mL each), sealed and marked. The samples were cryopreserved at -18 ° C.

7 Analysis steps

8 Results are calculated and expressed

The results of liquid chromatography-tandem mass spectrometry were quantified by standard curve method. The quantitative results of standard curve method were calculated according to formula (1) Xi = ci × (1) M 1000 where.

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

Ci - the concentration of the solution to be measured from the standard curve, in micrograms per milliliter (µg/mL);

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

M - The weight of the sample represented by the sample solution, in grams (g) (the wine is mL).

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 D.

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 E.

10% limit and recovery rate

12 Sec. Sec. Secancourt

13 Azathione Sulfonamide cyprodinil 0.24 Methanol 0.07 14 sulton buturon 2.98 methanol 0.90 15 bisacyl chloride carbetamide 1.22 methanol 0.36 16 pirimicarum pirimicarb 0.06 methanol 0.02

17 Isosubicin clomazone 0.14 Methanol 0.04 18 cyanocobalt cyanazine 0.06 methanol 0.02

19 Promised net prometryne 0.06 methanol 0.02

20% paraoxon methyl 0.26 methanol 0.08 21 4,4-dichlorobenzophenone a 4,4-dichlorobenzophenone 4.54 Methanol 1.36 22 thiacloprid 0.12 methanol 0.04 23 imidacloprid 7.34 Methanol 2.20 24 sulfothiazide ethidimuron 0.50 methanol 0.15

25 Butoxalone isomethiozin 0.36 Methanol 0.11 26 oat enemy diallate 29.74 methanol 8.92

27 Acetochlor 15.80 Methanol 4.74 28 nitrilpyram 5.70 methanol 1.71 29 caustic sorbitan methoprotryne 0.08 methanol 0.02 30 xylenolide dimethenamid 1.44 methanol 0.43

31 Terracuria terrbucarb 0.70 Methanol 0.21 32 tebuconazole penconazole 0.66 methanol 0.20 33 myclobose myclobutanil 0.34 methanol 0.10

34 Paclobutrazole paclobutrazol 0.20 Methanol 0.06 35 times thiophosphor sulfoxide fenthion sulfoxide 0.10 methanol 0.03 36 triazole alcohol triadimenol 3.52 methanol 1.06

37 Zhong Ding Ling butralin 0.64 Methanol 0.19

38 Spiroxamine 0.02 Methanol 0.01

39 Methylphenol tolclofos methyl 22.18 Methanol 6.66 40 beetin desmedipham 1.34 methanol 0.40

41 Pomperide methidathion 3.56 Methanol 1.07

42 Allyl alcohol allethrin 20.14 Methanol 6.04

43 Diazinon 0.24 Toluene 0.07 44 insecticides edifenphos 0.26 methanol 0.08

45 Propoxamine pretilachlor 0.12 Methanol 0.03

Table A.1 (continued)

Serial number Chinese name English name the limit of quantitation/(Mg/kg) Solvent Mix the standard solution Concentration/(mg/L)

46 Fluorosiliconazole flusilazole 0.20 Methanol 0.06

47 Propane Zinc iprovalicarb 0.78 Methanol 0.23 48 wheat rust Ling benodanil 1.16 methanol 0.35 49 fluoroamide flutolanil 0.38 methanol 0.11

50 Frozen Phosphorus famphur 1.20 Methanol 0.36

51 Benzoprene benalaxyl 0.42 Methanol 0.12 52 benzyl chlorotriazole alcohol diclobutrazole 0.16 methanol 0.05

53 Acetazole etaconazole 0.60 Methanol 0.18

54 Chlorophenylpyrimidinol fenarimol 0.20 Methanol 0.06 55 phthalic acid phthalic acid, dicyclobexyl ester 0.66 methanol 0.20

56 Tetramethrin tetramethirn 0.60 Methanol 0.18 57 antibacterial spirit dichlofluanid 0.86 toluene 0.26 58 solution grass cloquintocet mexyl 0.62 methanol 0.19

59 Biphenyltriazole alcohol bitertanol 11.14 Methanol 3.34 60 methyl chlorpyrifos chlorprifos methyl 5.34 methanol 1.60 61 pyranosone tepraloxydim 4.06 methanol 1.22

62 Methyl thiophanate methyl 13.34 methanol 2.00

Phosphorus Azinphos ethyl 36.30 Methanol 10.89 64 ethynyl oxalate clodinafop propargyl 1.62 methanol 0.24

65 Klebsuri triflumuron 1.30 Methanol 0.39 66 isoxazolone isoxaflutole 1.30 methanol 0.39 67 thiophanat ethyl 13.44 methanol 2.02

68 Quizalofop-ethyl 0.22 Methanol 0.07

69 Fiprofenamate Haloxyfop-methyl 0.88 Methanol 0.26 70 glazaprolone fluazifop butyl 0.08 methanol 0.03

71 Ethyl bromothiophosphorus bromophos-ethyl 189.24 Methanol 56.77

72 Scavenging bensulide 11.40 Methanol 3.42 73 ether benzenesulfuron triasulfuron 0.54 methanol 0.16 74 bromophenylene phosphate bromfenvinfos 1.00 methanol 0.30

75 Azoxystrobin 0.16 Methanol 0.05

7 Pyridobacillus pyrazophos 0.54 Methanol 0.16

77 Fipronil flufenoxuron 1.06 Methanol 0.32

78 Indoxacarb 2.52 methanol 0.75

Amino-avermectin benzene Formate Emamectin benzoate 0.10 Methanol 0.03 Group B 80 ethylene thiourea 17.40 methanol 5.22

81 Butyric acid hydrate daminozide 0.86 Methanol 0.26 82 cotton Long dazomet 42.34 methanol 12.70 83 nicotine 0.74 methanol 0.22 84 non-grass long fenuron 0.34 methanol 0.10

85 Methionine cyromazine 4.82 Methanol 0.72 86 rat death crimidine 0.52 methanol 0.16

87 Acephate Acephate 4.44 Methanol 1.33 88 grasses enemy molinate 0.70 methanol 0.21

89 Carbendazim 0.16 methanol 0.05

6-chloro-4-hydroxy-3-phenyl Pyridazine 6-chloro-4-hydroxy-3-phenyl-pyridazin 0.56 methanol 0.17

91 Propoxur 8.14 Methanol 2.44 92 isoxon isouron 0.14 methanol 0.04

93 Chlorotoluron 0.20 Methanol 0.06

94 Long effect Granule thiofanox 52.34 methanol 15.70

Table A.1 (continued)

Serial number Chinese name English name the limit of quantitation/(Mg/kg) Solvent Mix the standard solution Concentration/(mg/L)

95 Chlorobenzene chlorbufam 61.00 Methanol 18.30

96 Worms bendiocarb 1.06 Methanol 0.32

97 Fighting Chin propazine 0.10 Methanol 0.03 98 tert-butyl terbuthylazine 0.16 methanol 0.05

99 Diuron 0.52 methanol 0.16

100 Chloromethylthiophosphate chlormephos 149.34 Methanol 44.80

101 Moisturizer Pyorin 0.18 Methanol 0.06 102 wild Yan dry difenzoquat-methyl sulfate 0.28 methanol 0.08 Benzothiazide 17.00 Methanol 6.30

104 Acetylbenzoacetate pronamide 5.12 Methanol 1.54 105 dimethamine dimethachlor 0.64 methanol 0.19

106 Bromoguron Metobromuron 5.62 Toluene 1.68 107 phorate phytate 104.66 methanol 31.40 108 benzoate aclonifen 8.06 methanol 2.42 109 dean phosphorus mephosfolan 0.78 methanol 0.23

110 Benzylimidazole imibenzonazole-des-benzyl 2.08 Methanol 0.62 111 grass less long neburon 2.36 methanol 0.71

112 Aroma cream mefenoxam 0.52 Methanol 0.15 113 thiophosphate prothoate 1.64 methanol 0.25 114 ethofume sate 124.00 methanol 37.20 115 different rice blast net iprobenfos 2.76 methanol 0.83

116 Tepu TEPP 6.94 Methanol 1.04

117 Ciproazoleazole cyproconazole 0.24 Methanol 0.07 118 thiamethoxam 11.00 methanol 3.30

119 Feeding phosphorus crufomate 0.18 Methanol 0.05 120 spiramide etrimfos 12.50 methanol 1.88

121 Klebsilk coumatetralyl 0.46 Methanol 0.14 Spodophosphate cythioate 26.66 Methanol 8.00 123 phosphamine phosphamidon 1.30 methanol 0.39 124 beetin phenmedipham 1.50 methanol 0.45

125 Bentonate Bifenazate 7.60 Methanol 2.28 Carbamate fenhexamid 0.32 methanol 0.09 Albazole alcohol flutriafol 2.86 Methanol 0.86 128 antibacterial propyl alcohol furalaxyl 0.26 methanol 0.08 129 bio-allyrin bioallethrin 66.00 methanol 19.80 130 benzonitrile phospho...