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GB 23200.21-2016: Food safety national standard -- Determination of gibberellic acid residues in fruits by liquid chromatography-mass spectrometry / mass spectrometry
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Food safety national standard -- Determination of gibberellic acid residues in fruits by liquid chromatography-mass spectrometry / mass spectrometry
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GB 23200.21-2016
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Basic data | Standard ID | GB 23200.21-2016 (GB23200.21-2016) | | Description (Translated English) | Food safety national standard -- Determination of gibberellic acid residues in fruits by liquid chromatography-mass spectrometry / mass spectrometry | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 11,119 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 0350-2012 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.21-2016: Food safety national standard -- Determination of gibberellic acid residues in fruits by liquid chromatography-mass spectrometry / mass spectrometry
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Food safety national standards - Determination of gibberellic acid residues in fruits by liquid chromatography - mass spectrometry/mass spectrometry
National Standards of People's Republic of China
GB
Replace SN 0350-2012
National standards for food safety
Determination of Gibberellin Residue in Fruits
Liquid chromatography - mass spectrometry/mass spectrometry
National food safety standards-
Determination of gibberellic acid residue in fruit
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 0350-2012 "Determination of Gibberellin Residue in Import and Export Fruits by Liquid Chromatography-Mass Spectrometry/Mass Spectrometry".
Compared with SN/T 0350-2012, 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 fruit" to "fruit".
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN/T 0350-2012.
National standards for food safety
Determination of gibberellic acid residues in fruits by liquid chromatography - mass spectrometry/mass spectrometry
1 Scope
This standard specifies the preparation of gibberellic acid residues in fruit and the method of liquid chromatography-mass spectrometry/mass spectrometry.
This standard applies to the import and export of apples, oranges, peaches, pears and grapes in the detection of gibberellic acid residues, 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 residual gibberellic acid was extracted with acetonitrile, and the extract was purified by liquid-liquid distribution and then determined by 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 (C2H3N). Chromatographic pure.
4.1.2 Methanol (CH4O). Chromatographic purity.
4.1.3 Ethyl acetate (C4H8O2). Chromatographic purity.
4.1.4 Formic acid (CH2O2). Chromatography grade.
4.1.5 Potassium dihydrogen phosphate (K2HPO4).
4.1.6 Sodium hydroxide (NaOH).
4.1.7 Sulfuric acid (H2SO4).
4.1.8 Sodium chloride (NaCl).
4.2 solution preparation
4.2.1 sulfuric acid aqueous solution (pH2.5). 1 drop of sulfuric acid into 100 mL of water, adjust the water pH of 2.5.
4.2.2 Phosphate Buffer Solution (pH 7). 6.7 g of potassium dihydrogen phosphate and 1.2 g of sodium hydroxide were dissolved in 1 L of water.
4.2.3 0.15% formic acid solution. Remove 0.15 mL of formic acid and dilute to 100 mL with water.
4.3 standards
4.3.1 gibberelic acid standard (gibberellic acid, CAS NO. For 77-06-5, C19H22O6). purity ≥ 98%.
4.4 standard solution preparation
4.4.1 gibberellic acid standard stock solution. Weigh the appropriate amount of standard, dissolved in methanol, the solution concentration of 100 μg/mL. 0 ° C ~ 4 ° C refrigerated
Light preservation. Valid for three months.
4.4.2 Standard working solution. Standard stock solution is diluted to 4, 5, 10, 100 and 150 ng/mL with a blank sample solution as required
Standard working solution, equivalent to 8 μg/kg, 10 μg/kg, 20 μg/kg,.200 μg/kg, 300 μg/kg gibberellic acid in the sample. Pro
Prepare before use.
4.5 Materials
4.5.1 Organic phase microporous membrane. 0.45 μm.
5 instruments and equipment
5.1 Liquid Chromatography-Mass Spectrometry/Mass Spectrometer. Equipped with electrospray ion source.
5.2 Analysis of the balance. Analysis of balance. 0.01 g and 0.0001 g.
5.3 pH meter.
5.4 Rotary Evaporator.
5.5 vortex mixer.
5.6 Centrifuge. 4 000 r/min.
6 Preparation and storage of samples
A typical sample of about 500 g was taken from all the samples taken. The sampling site was carried out according to GB 2763 Appendix A, pulverized with a pulverizer,
Mixed evenly, are divided into two copies, respectively, into the clean container as a sample, sealed, and marked mark. The sample was stored at -18 ° C.
During sample and sample preparation, contamination of the sample or changes in the residue content should be prevented.
7 measurement steps
7.1 Extraction
Weigh 5 g of sample (accurate to 0.01 g) in a 50 mL plastic centrifuge tube, add 25 mL of acetonitrile and 2 g of sodium chloride, vortex for 1 min,
Centrifuged at 4 000 r/min for 5 min, the upper layer of acetonitrile extract transferred to the concentrated flask, the lower solution and then 20 mL of acetonitrile extraction time,
And acetonitrile extract, in 45 ℃ below the water bath under reduced pressure to near dry, with 10 mL of sulfuric acid aqueous solution to the residue transferred to 50 mL plastic centrifuge tube,
Add 20 mL of ethyl acetate, vortex for 1 min, centrifuge at 4 000 r/min for 5 min, transfer to another 50 mL plastic centrifuge tube,
Add 20 mL of ethyl acetate, repeat the above operation, combined with ethyl acetate extract, add 10 mL of phosphate buffer solution, vortex to 4 000
R/min centrifugal 5 min, take the phosphate buffer salt solution, ethyl acetate layer and then add 10 mL phosphate buffer solution extraction, combined
Phosphate buffer solution, add 50% sulfuric acid solution to adjust the solution pH 2.5 ± 0.2, add 20 mL of ethyl acetate, vortex 1 min to 4 000
R/min centrifugation 5 min, the upper layer of ethyl acetate transferred to the concentration of the bottle, phosphate buffer salt solution layer by adding 20 mL of ethyl acetate extraction
Once, combined with ethyl acetate extract in 45 ℃ below the water bath under reduced pressure to near dry, add 10.0 mL of methanol - water (1 1, volume ratio) dissolved
The residue was mixed and passed through a 0.45 m filter for liquid chromatography-mass spectrometry/mass spectrometry.
7.2 Determination
7.2.1 Liquid Chromatography-Mass Spectrometry/Mass Spectrometry
The reference conditions for liquid chromatography-mass spectrometry/mass spectrometry are as follows.
A) Column. C18 column, 150 mm × 4.6 mm (id), 5 μm or equivalent;
B) mobile phase. acetonitrile - 0.15% formic acid aqueous solution (35 65, volume ratio);
C) Flow rate. 0.4 mL/min;
D) Injection volume. 30 μL;
E) ion source. electrospray ion source;
F) scanning method. negative ion scanning;
G) Detection method. multiple reaction monitoring;
H) atomization gas, air curtain gas, auxiliary gas, collision gas are high purity nitrogen; before use should adjust the gas flow so that the mass spectral sensitivity of
To the test requirements, see Appendix A Table A.1 for reference conditions;
7.2.2 Determination by liquid chromatography-mass spectrometry/mass spectrometry
According to the content of gibberellic acid in the sample solution, the standard working solution with suitable response value is selected for chromatographic analysis, and the standard working fluid should have five
Concentration level. The response value of gibberellicate in the sample solution should be within the working curve of the instrument. Under the above chromatographic conditions, gibberellic acid
Of the reference retention time is about 4.9 min. The selective ion flow diagram of the standard solution is shown in Appendix B, Figure B.1.
7.2.3 Confirmation by liquid chromatography-mass spectrometry/mass spectrometry
According to the above conditions to determine the sample and the standard working fluid, if the detection of the quality of the peak retention time consistent with the standard working fluid, allowing partial
The relative abundance of the qualitative ion pair is consistent with the relative abundance of the standard working fluid, and the relative abundance is not allowed
In Table 1, it is judged that there is a corresponding analyte in the sample.
Table 1 Maximum allowable deviation of relative ion abundance when qualitative confirmation
Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10%
Allowable relative deviation ± 20% ± 25% ± 30% ± 50%
7.3 blank test
In addition to no sample, according to the above steps.
8 results are calculated and expressed
Use the chromatographic data processor or according to formula (1) to calculate the residual content of gibberellic acid in the sample, the calculation results need to deduct the blank value.
VCi
X (1)
Where.
X - the amount of gibberellic acid in the sample, in micrograms per kilogram (g/kg);
Ci - the concentration of gibberellicate from the standard curve in nanograms per ng (ng/mL);
V - the final volume of the sample solution in milliliters (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 reproducibility and its arithmetic mean (percentage) shall be in accordance with
Appendix D 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 E requirements.
10% limit and recovery rate
10.1 Quantitation limits
The quantification limit of this method is 10 μg/kg.
10.2 Recovery rate
See Appendix C for the recovery rates at different addition levels.
Appendix A
(Informative)
API 4000 LC-MS/MS system electrospray ion source reference conditions
Monitor ion pair and voltage parameters
A) electrospray voltage (IS). - 4500 V;
B) Atomizing gas pressure (GS1). 241.15 kPa (35 psi);
C) air curtain gas pressure (CUR). 172.25 kPa (25 psi);
D) Auxiliary gas flow rate (GS2). 310.05 kPa (45 psi);
E) ion source temperature (TEM). 550 ° C;
F) collision gas (CAD). 6;
G) ion pair, unwinding voltage (DP), collision gas energy (CE) and collision chamber outlet voltage (CXP) See A.1.
Table A.1 Ion pair, de-cluster voltage, collision gas energy and collision chamber outlet voltage
Non-Commercial Notices. The parameters listed in Appendix B are done at the API 4000 mass spectrometer, where the test instrument model is listed only for
Provide reference, does not involve commercial purposes, encourage standard users to try different manufacturers and models of equipment.
Name parent ion
M/z
Ion
M/z
Closing voltage (DP)
Collision gas
Energy (CE)
Collision chamber exit
Voltage (CXP)
Gamma
345.1
239.2 * -45 v-21
-11 v
143.2 -34
Note. "*" is a quantitative ion
Appendix B
(Informative)
Selective ion flow chart of gibberellic acid standard
Figure B.1 Selective ion flow chart of gibberellic acid (5 ng/mL) standard
Appendix C
(Informative)
Sample concentration and recovery of the experimental data
Table C.1 Experimental data on the concentration and recovery of the sample
Substrate Add Concentration/g/kg Recovery Range /% Precision Range /%
Apple 10 70.4 ~ 98.7 7.5
20 70.8 ~ 100.8 5.2
200 70.3 ~ 106.0 3.2
Orange 10 74.0 ~ 97.4 4.2
20 74.0 ~ 97.5 4.3
200 75.2 ~ 103.6 7.1
Peaches 10 71.6 ~ 99.3 13.7
20 73.8 ~ 102.8 10.5
200 71.6 ~ 103.0 12.6
Pear 10 70.4 ~ 109.0 5.3
20 73.3 ~ 102.2 8.8
200 73.7 ~ 101.0 5.7
Grape 10 70.2 ~ 98.3 13.0
20 70.3 ~ 98.1 9.4
200 70.0 to 102.0 8.9
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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