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GB 23200.20-2016: Food safety national standard -- Determination of abamectin residues in food by liquid chromatography-mass spectrometry / mass spectrometry
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Food safety national standard -- Determination of abamectin residues in food by liquid chromatography-mass spectrometry / mass spectrometry
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GB 23200.20-2016
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Basic data | Standard ID | GB 23200.20-2016 (GB23200.20-2016) | | Description (Translated English) | Food safety national standard -- Determination of abamectin residues in food by liquid chromatography-mass spectrometry / mass spectrometry | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 11,126 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 1973-2007 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.20-2016: Food safety national standard -- Determination of abamectin residues in food by liquid chromatography-mass spectrometry / mass spectrometry
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Food safety national standards - Determination of abamectin residues in food by liquid chromatography - mass spectrometry/mass spectrometry
National Standards of People's Republic of China
GB
Instead of SN/T 1973-2007
National standards for food safety
Determination of abamectin residues in food
Liquid chromatography - mass spectrometry/mass spectrometry
National food safety standards-
Determination of abamectin residue in foods
Liquid 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 1973-2007 "Determination of abamectin residues in food for import and export by high performance liquid chromatography-mass spectrometry/mass spectrometry
law".
Compared with SN/T 1973-2007, 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 1973-2007.
National standards for food safety
Determination of abamectin residues in food by liquid chromatography - mass spectrometry/mass spectrometry
1 Scope
This standard specifies the high performance liquid chromatography-mass spectrometry/mass spectrometry method for the determination of abamectin residues in food.
This standard applies to rice, garlic, spinach, apple, chestnut, tea, beef, lamb, chicken, fish, red peony, vinegar and
Determination of abamectin residues in honey, 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
Honey and vinegar samples were diluted with water and purified by C18 solid phase extraction column. Other samples were extracted with acetonitrile and treated with neutral alumina
Extraction column purification, high performance liquid chromatography - mass spectrometry/mass spectrometry, 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.
4.1 Reagents
4.1.1 acetonitrile. pure chromatography.
4.1.2 anhydrous sodium sulfate. 650 ℃ before burning 4 h, in the dryer to cool to room temperature, stored in a sealed bottle in reserve.
4.2 solution preparation
4.2.1 acetic acid aqueous solution (0.1%). take 1 mL of acetic acid, the volume of water to 1000 mL.
4.2.2 acetonitrile aqueous solution (16, V/V). take 100 mL of acetonitrile, add 600 mL of water, shake back.
4.3 standards
4.3.1 Avermectin standard substance. (Abamectin, C48H72O14, CAS No. 71754-41-2), abamectin B1a content is greater than
87%, the following abamectin content are avermectin B1a dollars.
4.4 standard solution preparation
4.4.1 abamectin standard stock solution. Weigh the appropriate amount (accurate to 0.0001 g) abamectin standard substance, acetonitrile dissolved in the preparation of the concentration
For 100 g/mL standard stock solution, stored in -18 ℃ refrigerator.
4.4.2 avermectin standard intermediate. accurate removal of avermectin standard stock solution, diluted with acetonitrile prepared with 1 g/mL concentration of the standard
Quasi-intermediate liquid. Store in 4 ℃ refrigerator.
4.4.3 abamectin standard working solution. according to the need to accurately remove the appropriate amount of avermectin standard intermediate, diluted with acetonitrile and set to the appropriate concentration
Degree of standard working fluid. Store in 4 ℃ refrigerator.
4.5 Materials
4.5.1 Neutral Alumina Solid Phase Extraction Column. 1000 mg, 3 mL.
4.5.2 C18 solid phase extraction column. 1000 mg, 6 mL.
4.5.3 Organic filter. 0.45 m.
5 instruments and equipment
5.1 High Performance Liquid Chromatography-Mass Spectrometry/Mass Spectrometer with Atmospheric Pressure Chemical Ionization Source (APCI Source)
5.2 Analysis of balance. 0.01 g and 0.0001 g
5.3 Homogenizer.
5.4 Centrifuge, 3000 r/min or more.
5.5 Vortex Oscillator.
5.6 solid phase extraction device.
5.7 Rotary Evaporator.
5.8 nitrogen blowing instrument.
6 Preparation and storage of samples
6.1 Preparation of the sample
6.1.1 apple, garlic, spinach, chestnut
Apple, chestnut. take the sample about 500 g, crushed with a crusher, into a clean container as a sample, sealed and do a good job; garlic,
Spinach. take the sample about 500 g, crushed with a mashed machine, into a clean container as a sample, sealed and do a good job.
6.1.2 rice, tea, red peony, vinegar
Take about 500 g of the sample and crush it all through a 850 μm sieve into a clean container as a sample, seal and mark it;
Vinegar can be packed in clean containers, sealed and marked.
6.1.3 beef, lamb, chicken, fish
Take a representative sample of about 500 g, crushed with a mashed machine, into a clean container as a sample, sealed and labeled.
6.1.4 honey
Take a representative sample of about 500 g, the amorphous sample will be forced to stir evenly, there are crystallization of the sample can be sealed after the sample cap,
Placed in a water bath of not more than 60 ℃, until the sample all dissolved and stir well, quickly cooled to room temperature. The prepared sample is packed in a clean container
Sealed and identified.
Note. The above sample sampling site according to GB 2763 Appendix A implementation.
6.2 Sample storage
Apple, garlic, spinach, chestnut and other samples at 0 ℃ 4 ℃ preservation; beef, lamb, chicken, fish and other samples at -18 ℃ to
Frozen under the preservation of rice, tea, red peony, vinegar, honey and other samples stored at room temperature.
During the operation of the sample preparation, the sample should be protected from contamination or changes in the content of the residue.
7 Analysis steps
7.1 Extraction
7.1.1 garlic, spinach, apple, chestnut, beef, lamb, chicken, fish samples
Accurately weigh 5 g (accurate to 0.01 g) homogeneous sample, add 5 g of anhydrous sodium sulfate and 15 mL of acetonitrile to 10,000 r/min
Homogenization 2 min, 3000 r/min centrifugation 5 min, the supernatant was filtered through anhydrous sodium sulfate and into the concentrated bottle. Re-use 10 mL of acetonitrile
Take the combined extract once. The extract was concentrated to 2 mL to 3 mL in a water bath at 40 ° C.
7.1.2 rice, tea leaves, red peony samples
Accurately weigh 5 g (accurate to 0.01 g) homogeneous sample, wet the sample with 2 mL of water (the tea is wet with 20 mL of water)
15 min, add 5 g of anhydrous sodium sulfate and 15 mL of acetonitrile to 10000 r/min homogeneous 2 min, 3000 r/min centrifugation 5 min,
The supernatant was transferred to a vial. With 10 mL of acetonitrile and then extracted once, the combined extract. The extract was concentrated to 2 at 40 ° C in a water bath
ML-3 mL.
7.1.3 Vinegar, honey samples
Accurately weigh 5 g (accurate to 0.01 g) homogeneous sample, add 30 mL of water and mix well.
7.2 Purification
7.2.1 rice, garlic, spinach, apple, chestnut, tea, beef, lamb, chicken, fish, red peony
The neutral alumina column was pre-leached with 3 mL of acetonitrile. The sample extracts obtained in 7.1.1 and 7.1.2 were transferred to neutral alumina
Column, the flask was washed twice with 5 mL of acetonitrile and the washing solution was transferred to a neutral alumina column. The flow rate was adjusted to about 1.5 mL/min.
2 mL of acetonitrile leach the column to collect the entire effluent. The effluent was dried at 50 ° C, the residue was dissolved in 1.00 mL of acetonitrile, filtered through a filter,
Determination by liquid chromatography - mass spectrometry/mass spectrometry.
7.2.2 Vinegar, honey samples
The C18 solid phase extraction column was pre-leached with 5 mL of acetonitrile and 5 mL of acetonitrile in water. Add the sample dilution obtained in 7.1.3
Into the C18 solid phase extraction column, adjust the flow rate of 1.5 mL/min or so, add 10 mL of water to wash C18 solid phase extraction column, the solid phase extraction column
dry. Add 5 mL of acetonitrile to elute and collect all eluent. The eluate was dried at 50 ° C, the residue was dissolved with 1.00 mL of acetonitrile,
Filtration, for liquid chromatography - mass spectrometry/mass spectrometry.
7.3 Determination
7.3.1 Liquid Chromatography - Mass Spectrometry/Mass Spectrometry Reference Conditions
A) Column. Column. C18 column, 150 mm × 2.1 mm (inner diameter), particle size 5 m.
B) Mobile phase. acetonitrile + acetic acid aqueous solution (0.1%) = 70 30.
C) Flow rate. 0.3 mL/min.
D) Column temperature. 40 ° C.
E) Injection volume. 20 μL.
F) ion source. atmospheric pressure chemical ionization source (APCI source), negative ion monitoring mode.
G) Mass Spectrometer Parameters. See Appendix A.
H) monitoring of ion pair (m/z). qualitative ion pair (872/565,872/854), quantitative ion pair (872/565).
7.3.2 Determination and confirmation of chromatography
According to the content of abamectin in the sample, the standard working solution with similar concentration was selected for chromatographic analysis. The peak area was determined by external standard method
Quantitative. The reference retention time of avermectin was 11.3 min under the above chromatographic conditions. Refer to Appendix B for the selection of the standard solution
Figure B.1, Figure B.2.
According to the above conditions to determine the sample and standard working fluid, if the detection of the quality of the peak retention time and standard working fluid consistent; qualitative
The relative abundance of the ion pair is consistent with the relative abundance of the standard working fluid at a considerable concentration, and the relative abundance deviation does not exceed the requirements in Table 1.
To determine the existence of the corresponding sample in the sample. The second-order spectrum of the standard solution is shown in Figure B.3 in Appendix B.
Table 1 qualitative relative ion abundance maximum allowable error
7.4 blank experiment
In addition to the sample, according to the above determination steps.
8 results are calculated and expressed
According to the data processing software processing or formula (1) to calculate the amount of abamectin residues in the sample.
MΑs
VCA
.. (1)
Where.
X - the amount of abamectin residues in milligrams per kilogram, mg/kg
A - the peak area of avermectin in the sample solution;
V - the final volume of the sample, in milliliters, mL;
As - avermectin standard working fluid peak area;
C - concentration of avermectin standard working solution in micrograms per milliliter, g/mL;
M - the final sample quality of the 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 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
10.1 Quantitation limits
The quantification limit of this method avermectin was 0.005 mg/kg.
10.2 Recovery rate
The recovery of avermectin is shown in Appendix C when the levels are 0.005 mg/kg, 0.01 mg/kg, 0.05 mg/kg.
Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10%
Allowable relative deviation ± 20% ± 25% ± 30% ± 50%
Appendix A
(Informative)
Mass spectrometer parameters 1)
A.1 Spray pressure. 60 psi.
A.2 Dry gas flow rate. 5 L/min.
A.3 Dry gas temperature. 350 ° C.
A.4 atmospheric pressure chemical ionization source evaporation temperature. 400 ℃.
A.5 Corona current. 10000 nA.
A.6 Capillary voltage. 3500 V.
1) Non-commercial statements. The listed parameters are performed on the Agilent LC-MSD-Trap-VL ion trap mass spectrometer, where the test instrument model is listed for reference only,
Does not involve commercial purposes, encourage standard users to try to use different manufacturers or models of equipment.
Appendix B
(Informative)
Selective ion chromatogram and secondary mass spectrum of standard solution
Figure B.1 Selective ion flow diagram of the avermectin reference substance (10 ng/mL) (565 m/z)
Figure B.2 Selective ion flow diagram of the avermectin reference substance (10 ng/mL) (854 m/z)
Figure B.3 Secondary spectrum of avermectin standard solution
Appendix C
(Informative)
Sample concentration and recovery of the experimental data
Sample concentration and recovery of the experimental data
sample name
Add concentration (mg/kg)
0.005 0.01 0.05
Rice 67.2% ~ 99.2% 74.6% ~ 90.8% 70.0% ~ 86.6%
Garlic 61.6% ~ 85.2% 63.2% ~ 83.4% 72.3% ~ 84.9%
Spinach 68.0% ~ 106.8 79.8% ~ 99.6% 81.7% ~ 96.1%
Apple 69.2% ~ 100.8% 76.6% ~ 107.6% 73.1% ~ 91.7%
Chestnut 78.1% ~ 111.2% 86.1% ~ 102.6% 72.6% ~ 83.6%
Tea 69.2% ~ 94.0% 74.8% ~ 85.8% 69.6% ~ 90.6%
Beef 61.2% ~ 95.6% 74.6% ~ 92.2% 74.1% ~ 99.1%
Lamb 66.0% ~ 76.8% 74.8% ~ 88.4% 68.3% ~ 79.7%
Chicken 64.4% ~ 85.6% 74.4% ~ 96.0% 80.4% ~ 101.3%
Fish 73.2% ~ 96.8% 74.6% ~ 103.6% 85.2% ~ 97.2%
Honey 74.0% ~ 97.2% 74.8% ~ 102.2% 66.6% ~ 87.3%
Red peony 64.8% ~ 85.2% 74.6% ~ 87.0% 70.9% ~ 96.9%
Vinegar 67.2% ~ 74.4% 65.6% ~ 87.8% 76.2% ~ 85.3%
Appendix D
(Normative appendix)
Laboratory repeatability requirements
Table D.1 Laboratory repeatability requirements
Measured component content
Mg/kg
Precision
0.001 36
> 0.01
> 1 14
Appendix E
(Normative appendix)
Inter-laboratory reproducibility requirements
Table E.1 Inter-laboratory reproducibility requirements
Measured component content
Mg/kg
Precision
0.001 54
> 0.01
> 1 19
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