Standard Briefing:Stadard ID: GB 23200.74-2016 Stadard Title: Food safety national standard -- Determination of Jinggangmycin Residue in Food by Liquid Chromatography -- Mass Spectrometry / Mass Spectrometry Price (USD): 239 Lead day (Deliver True-PDF English version): 3 days [Need to translate] Status: Valid
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Food safety national standard -- Determination of Jinggangmycin Residue in Food by Liquid Chromatography -- Mass Spectrometry / Mass Spectrometry
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GB 23200.74-2016
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Basic Data: Standard ID | GB 23200.74-2016 (GB23200.74-2016) | Description (Translated English) | Food safety national standard -- Determination of Jinggangmycin Residue in Food by Liquid Chromatography -- Mass Spectrometry / Mass Spectrometry | Sector / Industry | National Standard | Word Count Estimation | 12,143 | Date of Issue | 2016-12-18 | Date of Implementation | 2017-06-18 | Older Standard (superseded by this standard) | SN/T 2387-2009 | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of 2016 |
Contents, Scope, and Excerpt:GB 23200.74-2016
Food safety national standard - Determination of Jinggangmycin Residue in Food by Liquid Chromatography - Mass Spectrometry/Mass Spectrometry
GB
National standards for food safety
Determination of Jinggangmycin Residue in Food
Liquid chromatography - mass spectrometry/mass spectrometry
National food safety standards-
Determination of effectiveamycin 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
National Standards of People's Republic of China
Instead of SN/T 2387-2009
Preface
This standard replaces SN/T 2387-2009 "Determination of Jinggangmycin Residue in Import and Export Food by Liquid Chromatography-Mass Spectrometry/Mass Spectrometry".
Compared with SN/T 2387-2009, 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";
- "liquid chromatography - mass spectrometry/mass spectrometry" in the standard name to "liquid chromatography - tandem mass spectrometry";
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN/T 2387-2009.
National standards for food safety
Determination of Jinggangmycin Residue in Food by Liquid Chromatography - Mass Spectrometry/Mass Spectrometry
Scope
This standard specifies the method for the determination of Jinggangmycin residues in food by liquid chromatography-mass spectrometry/mass spectrometry.
This standard applies to rice, cabbage, onions, carrots, tomatoes, cucumbers, spinach, fungus, pear, lemon, almonds, tea, pork,
Pig liver, tilapia, shrimp in the detection and confirmation of Jinggangmycin 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 document.
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 of Jinggangmycin residues in methanol aqueous solution extraction, by HLB solid phase extraction column or ethyl acetate liquid extraction and purification, with liquid chromatography -
Mass spectrometry/mass spectrometer detection and confirmation, external standard method quantitative.
4 reagents and materials
Unless otherwise specified, the reagents used in this method are pure liquid chromatography, water in line with GB/T 6682 in the provisions of a water.
4.1 Reagents
4.1.1 Ammonium acetate (CH3COONH4, CAS number. 631-61-8).
4.1.2 Methanol (CH3OH, CAS No. 67-56-1).
4.1.3 Acetonitrile (CH3CN, CAS No. 75-05-8).
4.1.4 Ethyl acetate (CH3COOCH2CH3, CAS number. 141-78-6).
4.1.5 glacial acetic acid (CH3COOH, CAS number. 64-19-7).
4.2 solution preparation
4.2.1 methanol solution (9 1). the amount of 90 mL of methanol by adding 10 mL of water, mix.
4.2.2 5 mmol/L ammonium acetate buffer solution. Weigh 0.385 g of ammonium acetate, dissolved in water and fixed to 1 000 mL, adjusted with glacial acetic acid
PH to 4.5 ± 0.1.
4.3 standards
4,3.1 Jinggangmycin standard (Validamycin A, molecular formula. C20H35NO13, CAS. 37248-47-8). purity ≥ 91.0%.
4.4 standard solution preparation
4.4.1 Jinggangmycin standard stock solution. Weigh 2 mg (accurate to 0.1 mg) the standard of Jinggangmycin, dissolved in water and set to
25 mL of a brown volumetric flask to prepare a standard stock solution at a concentration of 80 mg/L.
4.4.2 Jinggangmycin matrix standard working solution. according to the need, with blank samples in accordance with the sample treatment steps to get the extract, preparation is not
With the concentration of the matrix standard solution, is now available.
4.5 Materials
4.5.1 HLB column. 6 mL /.200 mg or equivalent; activated with 6 mL of methanol and 6 mL of water before use.
4.5.2 Filtration. 0.22 m, biphasic.
5 instruments and equipment
5.1 Liquid Chromatography - Mass Spectrometry/Mass Spectrometer. Atmospheric Pressure Chemical Ionization Source (APCI).
5.2 Analysis of balance. 0.01 g and 0.0001 g.
5.3 vortex mixer.
5.4 Homogenizer.
5.5 Centrifuge. speed greater than 3 000 r/min.
5.6 nitrogen blowing concentrator.
5.7 Centrifuge tube. 50 mL Teflon centrifuge tube and 50 mL stopper glass centrifuge tube.
5.8 scale tube. 30 mL, the smallest scale of 0.1 mL.
5.9 pH meter. the amount of 0.1.
6 Sample preparation and storage
6.1 Sample requirements
During sample preparation, the sample should be protected from contamination or changes in residue content.
6.2 Tea and cereals
Approximately 500 g of the representative sample, ground and ground through the mill and passed through a 2.0 mm round hole screen, mixed and sealed in a clean container.
Remember, stored at 0 ℃ ~ 4 ℃ refrigerated.
6.3 vegetables and fruits
To replace the sample of about 500 g, chopped, the multi-functional food mixer fully mashed evenly, into a clean container sealed, marked mark,
Frozen at -18 ℃ below the storage.
6.4 nuts
Approximately 500 g of the sample was taken and ground thoroughly with an attritor and passed through a 20 mm round hole screen, mixed, sealed in a clean container, marked with a mark,
Store at 0 ℃ ~ 4 ℃.
6.5 animal muscle, liver, fish, shrimp
Replace the sample part of about 500 g, chopped, by the multi-functional food mixer fully mashed evenly, into a clean container sealed, marked
Note, in -18 ℃ below the frozen storage.
Note. The above sample sampling site according to GB 2763 Appendix A implementation.
7 Analysis steps
7.1 Extraction
7.1.1 Rice, edible fungus, almonds
Weigh 2.5 g sample (accurate to 0.01 g), placed in 50 mL polytetrafluoroethylene centrifuge tube, add 20 mL of methanol solution, with homogenizer high
Rapid homogenate extraction 2 min, 3 000 r/min centrifugation 5 min, collecting supernatant in a scale tube. The residue after centrifugation was dissolved in 5 mL of methanol
The supernatant was combined once the above extraction step was repeated and the nitrogen was concentrated to 2.5 mL below the nitrogen bath at 45 ° C to be purified.
7.1.2 cabbage, onions, carrots, tomatoes, cucumber, spinach, pear, lemon, pork, liver, fish, shrimp
Weigh 2.5 g sample (accurate to 0.01 g), placed in 50 mL polytetrafluoroethylene centrifuge tube, add 20 mL of methanol, homogenizer high speed uniform
Pulp extraction 2 min, 3 000 r/min centrifugation 5 min, collecting supernatant in a scale tube. The residue after centrifugation was diluted with 5 mL of methanol solution
Repeat the above extraction step 1, the supernatant, in 45 ℃ water bath blowing nitrogen concentrated to 2.5 mL below, to be purified.
7.1.3 Tea
Weigh 1 g of sample (accurate to 0.01 g), add 1.5 mL of water, mix, and the rest according to 7.1.1.
7.2 Purification
7.2.1 Solid phase extraction (SPE) purification
The resulting solution from 7.1 was transferred to a pretreated HLB solid phase extraction column and the sample solution was passed through solid phase extraction at a flow rate of about 1 drop/s
Column, rinse the column with 2 mL of water, collect all the effluent and eluent to a scale tube, add water to a volume of 5.00 mL, mix, over 0.22 m
Filter for determination.
7.2.2 liquid - liquid distribution purification
The resulting solution in 7.1 was fixed to 5.00 mL with water, mixed into a 50 mL stoppered glass centrifuge tube, 5 mL of ethyl acetate was added,
Vortex oscillation 3 min, 3 000 r/min centrifugal 5 min, discard the upper ethyl acetate phase, and then 5 mL ethyl acetate repeated operation once. Too
0.22 m filter for liquid chromatography-tandem mass spectrometry.
7.3 Determination
7.3.1 Liquid Chromatographic Reference Conditions
Column. HILIC (250 mm × 4.6 mm, particle size 5 m), or equivalent.
Mobile phase. acetonitrile 5 mmol/L ammonium acetate buffer solution, gradient elution (see Table 1).
Flow rate. 1 000 L/min.
A) Column temperature. 35 ° C.
B) Injection volume. 10 μL.
Table 1 Gradient elution conditions for liquid chromatography
Time/min 5 mmol/L ammonium acetate buffer solution /% acetonitrile /%
0.0 20 80
4.0 45 55
10.0 45 55
10.1 20 80
16.0 20 80
7.3.2 Mass spectrometry reference conditions
See Appendix A for the mass spectrometric conditions.
7.3.3 Determination and confirmation of chromatography
Under the optimum working condition of the instrument, according to the content of the compound in the sample solution, the substrate standard working solution with similar peak height is selected,
Quality standard working solution and sample solution volume measurement. With the peak area as the ordinate, the concentration of abscissa to draw the standard working curve, with
The standard working curve is used to quantify the sample, and the response values of the test compound to be tested in the working solution and the sample solution should be measured linearly
Within range. In the above instruments, the reference retention time of Jinggangmycin is about 8.10 min; the calibration curve for the calibration product of Jinggangmycin is given in Appendix
B Figure B.1.
Table 2 in the same experimental conditions, the sample solution to be tested material retention time, and the matrix standard working solution retention time deviation of ± 2.5%
And the relative abundance of the qualitative ion pairs in the sample solution is compared with the matrix standard working solution close to the concentration. The deviation does not exceed the standard
It is determined that there is a corresponding analyte in the sample.
Table 2 Maximum allowable deviation of relative ion abundance using liquid chromatography-mass spectrometry/mass spectrometry
Relative ion abundance 50% 20% to 50% 10% to 20% 10%
Permissible relative deviation 20% 25% 30% 50%
7.4 blank test
In addition to the sample, according to the above determination steps.
8 results are calculated and expressed
Using the external standard method, according to formula (1) to calculate the sample of Jinggangmycin residues, the results should be deducted blank value.
Vc
X (1)
Where.
X - the amount of Jinggangmycin residues in micrograms per kilogram (g/kg);
C - the concentration of the component to be measured in the sample from the standard working curve, in micrograms per liter (g/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 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 limit of quantification of this method was 10 μg/kg.
10.2 Recovery rate
When adding levels of 10 μg/kg, 25 μg/kg, 50 μg/kg, the recovery rates of Jinggangmycin in different substrates are given in Appendix C.
Appendix A
(Informative)
Reference to mass spectrometry conditions
Reference mass spectrometry conditions.
A) Ionization mode. Atmospheric pressure Chemical ionization positive ion mode (APCI).
B) Mass Spectrometry. Multiple Reaction Monitoring (MRM).
C) Resolution. Unit resolution.
D) air curtain gas pressure (CUR). 207 KPa (nitrogen).
E) Corona discharge current (NC). 5.00 μA.
F) Atomization temperature (TEM). 600 ° C.
G) Atomizing gas pressure. 138 KPa (nitrogen).
H) Impact air pressure (CAD). 34.5 KPa (nitrogen).
I) Other mass spectral parameters are shown in Table A.1.
Table A.1 Main reference mass spectrometry parameters
Compounds
Ion pair
(M/z)
Dwell time
Ms
To cluster voltage
(DP)/V
Inlet voltage
(EP)/V
Collision energy
(CE)/eV
Collision cell outlet voltage
(CXP)/V
Jinggangmycin
498.3/336.3 100 75 3 31.74 12.08
498.3/178.1a 100 75 3 38.57 12.08
498.3/142.2 100 75 3 48.77 12.08
Note. For different mass spectrometry instruments, the instrument parameters may be different, before the determination of the mass spectrometry parameters should be optimized to the best.
A ion pair is a quantitative ion pair
Appendix B
(Informative)
Standard multi-reaction monitoring (MRM) chromatograms
Figure B.1 Multi-reaction monitoring (MRM) chromatogram of Jinggangmycin standard solution
Ion pair 498.3/336.3
Ion pair 498.3/178.1
Ion pair 498.3/142.2
Appendix C
(Informative)
Addition Recovery of Jinggangmycin in Different Substrates
Table C.1 Recovery of Jinggangmycin in Different Substrates
Sample Concentration/μg/kg Recovery Range /% Sample Concentration/μg/kg Recovery Range /%
Rice
10 87.2 ~ 101.8
10 86.6 ~ 111.0
25 92.8 ~ 101.6 25 87.2 ~ 108.8
50 89.2 ~ 100.8 50 87.2 ~ 113.6
cabbage
10 96.8 to 109.4
lemon
10 86.2 to 111.6
25 94.4 ~ 108.0 25 89.6 ~ 102.4
50 96.0 ~ 108.0 50 87.6 ~ 106.8
10 94.6 ~ 108.4
almond
10 90.6 ~ 105.4
25 93.6 ~ 109.6 25 87.2 ~ 111.2
50 93.6 ~ 108.0 50 99.6 ~ 113.2
carrot
10 91.6 ~ 109.2
tea
10 86.0 to 107.8
25 91.2 ~ 105.6 25 87.2 ~ 106.4
50 91.2 ~ 108.4 50 86.8 ~ 104.0
tomato
10 91.6 ~ 107.2
pork
10 89.4 ~ 105.6
25 91.2 ~ 111.2 25 87.2 ~ 108.0
50 94.8 ~ 111.6 50 88.0 ~ 101.6
cucumber
10 98.6 ~ 111.4
Liver
10 90.0 to 106.4
25 89.6 ~ 108.8 25 92.0 ~ 106.4
50 95.2 ~ 111.6 50 87.2 ~ 106.4
spinach
10 87.0 ~ 104.2
Tilapia
10 88.8 ~ 107.2
25 92.8 ~ 108.8 25 96.8 ~ 112.8
50 89.6 to 108.0 50 88.4 to 113.2
Fungus
10 92.8 to 107.2
10 93.4 ~ 106.2
25 92.8 ~ 109.6 25 93.6 ~ 113.6
50 89.2 ~ 108.8 50 88.0 ~ 112.0
IX
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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