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GB 29708-2013: Determination of Sodium Pentachlorophenol residues in animal derived food by Gas Chromatography-mass Spectrometric method
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Determination of Sodium Pentachlorophenol residues in animal derived food by Gas Chromatography-mass Spectrometric method
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GB 29708-2013
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Basic data
| Standard ID | GB 29708-2013 (GB29708-2013) |
| Description (Translated English) | Determination of Sodium Pentachlorophenol residues in animal derived food by Gas Chromatography-mass Spectrometric method |
| Sector / Industry | National Standard |
| Classification of Chinese Standard | C53 |
| Classification of International Standard | 67.020 |
| Word Count Estimation | 11,137 |
| Quoted Standard | GB/T 6682; GB/T 1.1-2000 |
| Adopted Standard | GB/T 6682; GB/T 1.1-2000 |
| Regulation (derived from) | China Food & Drug Administration [2013] No. 234, November, 1, 2013 |
| Issuing agency(ies) | Ministry of Agriculture of the People's Republic of China, National Health and Family Planning Commission of the People's Republic of China |
| Summary | This standard specifies the animal-derived food sodium pentachlorophenol residue detection sample preparation and gas chromatography mass spectrometry. |
GB 29708-2013: Determination of Sodium Pentachlorophenol residues in animal derived food by Gas Chromatography-mass Spectrometric method
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Determination of Sodium Pentachlorophenol residues in animal derived food by Gas CHromatography-mass Spectrometric method
National Standards of People's Republic of China
National Food Safety Standard
Determination of the residues in animal foods, sodium pentachlorophenol
Gas chromatography - mass spectrometry
Published 2013-09-16
2014-01-01 implementation
Ministry of Agriculture, People's Republic of China
National Health and Family Planning Commission People's Republic of China released
National Food Safety Standard
Determination of the residues in animal foods, sodium pentachlorophenol
Gas chromatography - mass spectrometry
1 Scope
This standard specifies the sample preparation and gas chromatography-mass spectrometry in animal foods sodium pentachlorophenol residues detected.
This standard applies to porcine muscle, sodium pentachlorophenol residues in chicken liver and kidneys and muscle and liver tissue detection.
2 Normative references
The following documents for the application of this document is essential. For dated references, only applies to the version dated paper
Pieces. For undated references, the latest edition (including any amendments) applies to this document.
GB/T 6682 Water for analytical laboratory specifications and test methods
Principle 3
The sample of residual sodium pentachlorophenol, trichloroacetic acid precipitated protein, cyclohexane - ethyl acetate solution was extracted, acetic anhydride - pyridine derivative,
Gas Chromatography - Mass Spectrometry, external standard.
4 Reagents and materials
The following reagents used, unless otherwise stated were of analytical reagent; water as a water line with GB/T 6682 provisions.
4.1 sodium pentachlorophenol Standard. content ≥98.0%.
4.2 potassium carbonate.
4.3 n-hexane.
4.4 cyclohexane.
4.5 ethyl acetate.
4.6 of acetic anhydride.
4.7 pyridine.
4.8 TCA.
4.9 concentrated hydrochloric acid.
4.10 5% trichloroacetic acid solution. Take acid solution 5g, dissolve and dilute to 100mL with water.
4.11 2.4mol/L hydrochloric acid solution. Take 20mL of concentrated hydrochloric acid was dissolved and diluted to 100mL with water.
4.12 cyclohexane - ethyl acetate. ethyl take 10mL, add cyclohexane 40mL, mix.
4.13 acetic anhydride - pyridine. acetic anhydride take 10mL, add pyridine 10mL, mix, now with the current.
4.14 0.2mol/L potassium carbonate solution. Take potassium carbonate 27.6g, dissolved and diluted with water to 1000mL.
4.15 1mg/mL standard stock solution pentachlorophenol sodium. sodium pentachlorophenol accurately weighed standard 10mg, in 10mL volumetric flask, and dissolved in water
Diluted to the mark, formulated at a concentration of 1mg/mL of stock standard solution of sodium pentachlorophenol. The following stored at -20 ℃, valid for three months.
4.16 2μg/mL sodium pentachlorophenol standard working solution. precise amount of 1mg/mL standard stock solution of sodium pentachlorophenol 200μL, in an amount of 100mL
Flask was diluted with water to the mark, formulated at a concentration of 2μg/mL of sodium pentachlorophenol working standard solution, now with the current.
5. Apparatus
5.1 gas chromatograph mass spectrometer. with the EI source.
5.2 Analytical balance. a sense of volume 0.00001g.
5.3 Balance. a sense of the amount of 0.01g.
5.4 high-speed centrifuge.
5.5 oscillator.
5.6 vortex mixer.
5.7 tissue homogenizer.
5.8 Nitrogen blowing instrument.
5.9 rotary evaporator.
5.10 centrifuge tube. 50mL.
Preparation and Storage of sample 6
6.1 Preparation of the sample
Fresh or thawed take appropriate blank or test tissue, minced, and homogenized.
--- homogeneous test sample taken, as the feed try.
--- the blank sample were homogeneous, as a blank sample.
--- blank sample taken homogeneous, standard working solution is added an appropriate concentration, is added as a blank sample.
Save 6.2 sample
-20 ℃ less storage backup.
Determination Step 7
7.1 Preparation of matrix-matched standard curve
Accurately taken 2μg/mL sodium pentachlorophenol appropriate amount of working standard solution, prepared with water to a concentration of 2,5,10,20,50,100μg/L series
Standard solution from each 1.0 mL, extracted separately dissolved, after drying 6 parts distilled white residue sample, mixed, dissolved with 2.4mol/L hydrochloric acid
PH was adjusted to less than 2.0, add cyclohexane - ethyl acetate solution 5mL, vortexed, 8000r/min centrifugal 10min, the organic layer was pipetted and then
Adding cyclohexane - ethyl acetate solution 5mL, the organic layer was twice vortex mixed, 8000r/min centrifugal 10min, combined, rotary evaporated at 45 ℃
dry. By derivatization steps, gas chromatography mass spectrometry. A characteristic ion mass chromatogram peak area for the vertical axis, the concentration control solution of
Abscissa, the standard curve. Seeking regression equation and correlation coefficient.
7.2 extract
Sample Weigh 5g ± 0.05g, in 50mL centrifuge tubes, add water 10mL, Vortex, 8000r/min centrifugal 10min, supernatant
Solution, 5% trichloroacetic acid was added 5mL, Vortex, 8000r/min centrifugal 10min, the supernatant was adjusted to pH with 2.4mol/L hydrochloric acid solution
To less than 2.0, add cyclohexane - ethyl acetate solution 5mL, vortexed, 8000r/min centrifugal 10min, the organic layer was pipetted, cyclohexyl plus
Alkoxy - ethyl acetate solution 5mL, vortexed, 8000r/min centrifugal 10min, the two organic layers were combined, rotary evaporated to dryness at 45 ℃.
7.3 derivatized
The residue was added cyclohexane - ethyl acetate, 1.0 mL, was added a small amount of anhydrous sodium sulphate, was added acetic anhydride - pyridine solution, 100 L, sealed and
60 ℃ reaction 15min, cooled and 0.5 mL potassium carbonate solution was added, mixed thoroughly, left to stand stratification, the organic phase, gas chromatography mass spectrometry.
7.4 Determination
7.4.1 Chromatographic conditions
7.4.1.1 Column. DB-5MS5% phenylmethyl polysiloxane (30m × 0.25mm, film thickness 0.25μm), or equivalent person.
7.4.1.2 Inlet temperature. 250 ℃.
7.4.1.3 Injection mode. splitless.
7.4.1.4 Injection volume. 2μL.
7.4.1.5 Column temperature. initial temperature 140 ℃, retention 2min, at 10 ℃/min was heated to 200 ℃, at 15 ℃/min was heated to 280 ℃, maintained
3.0min.
7.4.1.6 Carrier gas. Helium, 1.0mL/min (constant).
7.4.2 MS conditions
7.4.2.1 EI Source. 70eV.
7.4.2.2 Solvent delay. 3min.
7.4.2.3 GC/MS transfer line temperature. 280 ℃.
7.4.2.4 selected ion monitoring mode, detect ions Sim (m/z). 266,308,237,165,130.
7.4.2.5 quantitative ion. 266.
7.4.3 Assay
By retention time and the retention time of the standard solution sample chromatogram, the peaks corresponding to the characteristic ions of each standard concentration Chromatography
In contrast to the qualitative characteristics of ion peaks. Relative abundance compared to the relative abundance of ions in the sample solution with the matrix matching criteria ions in solution,
In accordance with Table 1. Matrix-matched standard solution and test solution was added mass chromatogram characteristic ions are given in Appendix A.
Table 1 sample solution ion relative abundance of the tolerance range
The relative abundance
Tolerance
> 50 ± 20
> 20 ~ 50 ± 25
> 10 ~ 20 ± 30
≤10 ± 50
7.5 Blank test
Measure the blank sample assay step is performed in exactly the same operation in parallel.
Calculation and Expression of Results 8
Single-point calibration.
c =
cSA
AS
(1)
Or matrix-matched standard curve calibrated by. AS = acS b to obtain a and b, then
c =
Ab
(2)
The specimens residual amount of sodium pentachlorophenol (μg/kg) (3) is calculated according to the formula.
X =
cV
(3)
Where.
C --- try to supply feed solution of pentachlorophenol sodium concentration, in units of nanograms per milliliter (ng/mL);
cS --- pentachlorophenol sodium concentration, expressed in nanograms per milliliter (ng/mL) in standard solution;
A --- try to supply feed solution of the peak area of sodium pentachlorophenol derivative;
--- the AS standard solution of sodium pentachlorophenol derivative peak area;
X-try for feed Residue --- sodium pentachlorophenol, in micrograms per kilogram (μg/kg);
The residue was V --- constant volume in milliliters (mL);
m --- try supply feed mass in grams (g).
Note. The blank value should be subtracted from the results, expressed as the arithmetic mean of the measurement result measured parallel to three significant figures.
9 detection sensitivity, accuracy and precision
9.1 Sensitivity
The detection limit of the method was 0.25μg/kg.
The limit of quantitation of the method, the muscle tissue was 0.5μg/kg, liver and kidney tissues was 1μg/kg.
9.2 Accuracy
In the process of muscle tissue 0.5μg/kg ~ 2μg/kg, liver and kidney tissues at 1μg/kg ~ 4μg/kg was added on the concentration level
Recoveries of 60% to 120%.
9.3 Precision
≤20% relative standard deviation in this method and inter - batch relative standard deviation of ≤20%.
Appendix A
Chromatogram
Figure A.1 standard solution wherein sodium pentachlorophenol ion mass chromatogram (2μg/L)
Figure A.2 wherein the sample blank pig liver tissue ion mass chromatogram
Figure A.3 pig liver tissue sample blank add characterized pentachlorophenol sodium ion mass chromatogram (1μg/kg)
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