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Determination of Diclazuril residues in edible tissue of chicken by High Performance Liquid Chromatographic method
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Basic data
| Standard ID | GB 29701-2013 (GB29701-2013) |
| Description (Translated English) | Determination of Diclazuril residues in edible tissue of chicken by High Performance Liquid Chromatographic method |
| Sector / Industry | National Standard |
| Classification of Chinese Standard | C53 |
| Classification of International Standard | 67.020 |
| Word Count Estimation | 9,917 |
| 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 Edible Chicken Tissues DICLAZURIL residue detection sample preparation, high-performance liquid chromatographic method. |
GB 29701-2013: Determination of Diclazuril residues in edible tissue of chicken by High Performance Liquid Chromatographic method
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Determination of Diclazuril residues in edible tissue of chicken by High Performance Liquid Chromatographic method
National Standards of People's Republic of China
National Food Safety Standard
Measured in grams of chicken edible tissues Diclazuril residues
High performance liquid chromatography
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
Measured in grams of chicken edible tissues Diclazuril residues
High performance liquid chromatography
1 Scope
This standard specifies the sample preparation and high performance liquid chromatographic method chicken edible tissues Diclazuril remaining amount detection.
This standard applies to chicken muscle, liver and kidney diclazuril residues detected.
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 specimens remaining diclazuril, extracted with acetonitrile, hexane degreasing, concentrated to dryness under reduced pressure, high performance liquid chromatography - UV determination, external standard
The statutory amount.
4 Reagents and Materials
The following reagents used, except those otherwise specified, reagents were of analytical grade; water as a water line with GB/T 6682 provisions.
4.1 Diclazuril reference. content ≥99%.
4.2 phosphoric acid.
4.3 n-hexane.
4.4 N, N- dimethylformamide.
4.5 Methanol. HPLC grade.
4.6 Acetonitrile. chromatographically pure.
4.7 0.2% phosphoric acid. phosphoric take 2.34mL, dissolved and diluted with water to 1000mL.
4.8 1mg/mL diclazuril standard stock solution. Weigh accurately Diclazuril reference substance 10mg, in 10mL flask, N, N- dimethyl
Formamide dissolved and diluted to the mark, formulated at a concentration of 1mg/mL of diclazuril standard stock solution. -20 ℃ less storage, effective
Period of 6 months.
4.9 10μg/mL diclazuril standard working solution. exact amount of 1mg/mL diclazuril standard stock solution 1.0mL, in an amount of 100mL
Bottle,, N-dimethylformamide was diluted to the mark with N, formulated at a concentration of 10μg/mL of diclazuril working standard solution, -20 ℃ to
Under Save, valid for three months.
5 instruments and equipment
5.1 HPLC. with UV detector.
5.2 Analytical balance. a sense of volume 0.00001g.
5.3 Balance. a sense of the amount of 0.01g.
5.4 rotary evaporator.
5.5 homogenizer.
5.6 high-speed centrifuge.
5.7 polypropylene centrifuge tube. 50mL.
5.8 eggplant-shaped bottle. 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.
--- the test sample taken after homogenization, as the feed try.
--- blank sample taken after homogenization, as a blank sample.
--- blank sample taken after homogenization, adding a suitable concentration of the standard working solution, is added as a blank sample.
Save 6.2 sample
Or less at -20 ℃.
Determination Step 7
7.1 Preparation of matrix-matched standard curve
The precise amount of diclazuril appropriate amount of working standard solution, 6 parts were added to the sample of the blank, to obtain a concentration of 100,250,500,
1000,2500 and 5000μg/kg of a matrix-matched standard solution series, according to the extraction steps for HPLC determination. With
Measured peak area for the vertical axis, corresponding to the concentration of standard solution as abscissa, the standard curve. Seeking regression equation and correlation coefficient.
7.2 extract
Sample Weigh 2g ± 0.02g, in 50mL polypropylene centrifuge tube, acetonitrile was added 10mL, homogeneous 1min, shaken for 15min,
6000r/min centrifugal 10min, extract was collected in 50mL acetonitrile eggplant-shaped flask, the residue was extracted once again repeated, the two extracts were combined,
Hexane 5mL, n-hexane layer was discarded, n-propanol was added 5mL, evaporated to dryness under reduced pressure at 50 deg.] C, mobile phase the residue was dissolved 1.0mL,
15000r/min centrifugal 10min, the supernatant for HPLC assay.
7.3 Determination
7.3.1 HPLC conditions
7.3.1.1 Column. C18 (250mm × 4.6mm, particle size 5μm), or equivalent person.
7.3.1.2 mobile phase. acetonitrile 0.2% phosphoric acid (5743, volume ratio).
7.3.1.3 flow rate. 1mL/min.
7.3.1.4 wavelength. 278nm.
7.3.1.5 Column temperature. 30 ℃.
7.3.1.6 Injection. The injection volume 20μL.
7.3.2 Assay
Take a sample solution and standard solutions corresponding, for single or multi-point calibration, by external standard method, the peak area is calculated. Standard solution and sample solution
Diclazuril was the response value should be within the linear range of the detection instrument. In the chromatographic conditions, the standard solution and blank sample solution added
HPLC Appendix A. FIG.
7.4 blank test
But without addition of the sample, the same steps employed in parallel operation.
Calculation and Expression of Results 8
Diclazuril the residual amount of the specimens (μg/kg) according to formula (1).
X =
A × cS × V
AS × m
(1)
Where.
--- for the residual amount of X-try feed diclazuril, in units of micrograms per kilogram (μg/kg);
A --- peak area of a sample of diclazuril;
cS --- standard concentration of diclazuril in units of micrograms per liter (μg/L);
V --- final sample volume in milliliters (mL);
AS --- standard solution peak area of diclazuril;
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 50μg/kg, the limit of quantitation of 250μg/kg.
9.2 Accuracy
This method of adding 250μg/kg ~ 2500μg/kg levels on recoveries of 70% to 120%.
9.3 Precision
The relative standard deviation of the method ≤20%, inter-assay relative standard deviation ≤20%.
Appendix A
Chromatogram
Figure A.1 Diclazuril chromatogram of the standard solution (100μg/L)
Figure A.2 chicken muscle tissue sample blank chromatogram
Figure A.3 blank Chicken muscle sample was added diclazuril chromatogram (250μg/kg)
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