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GB 29683-2013: Determination of Paracetamol residues in animal derived food by High Performance Liquid Chromatographic method
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Determination of Paracetamol residues in animal derived food by High Performance Liquid Chromatographic method
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GB 29683-2013
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Basic data | Standard ID | GB 29683-2013 (GB29683-2013) | | Description (Translated English) | Determination of Paracetamol residues in animal derived food by High Performance Liquid Chromatographic method | | Sector / Industry | National Standard | | Classification of Chinese Standard | C53 | | Classification of International Standard | 67.020 | | Word Count Estimation | 9,955 | | 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 acetaminophen residue detection sample preparation, high-performance liquid chromatographic method. This standard applies to pigs, cattle, sheep, chicken, liver the detection of drug residues. | GB 29683-2013: Determination of Paracetamol residues in animal derived food by High Performance Liquid Chromatographic method
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Determination of Paracetamol residues in animal derived food by High Performance Liquid Chromatographic method
National Standards of People's Republic of China
National Food Safety Standard
Determination of the amount of animal foods residual acetaminophen
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
Determination of the amount of animal foods residual acetaminophen
High performance liquid chromatography
1 Scope
This standard specifies the sample preparation and high performance liquid chromatographic method for animal food in an amount of acetaminophen residue detection.
This standard applies to pigs, cattle and sheep muscle, liver and kidney tissues acetyl detected residual amount of acetaminophen.
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
Remaining in a sample of acetaminophen, extracted with ethyl acetate, an HLB purification column, eluting with methanol, dried with nitrogen, dissolved in mobile phase, and efficient
Liquid chromatography, external standard.
4 Reagents and materials
The following reagents used, unless otherwise stated who were of analytical grade; water line with an aqueous GB/T 6682 provisions.
4.1 pairs of acetaminophen standard. content ≥99%.
4.2 Methanol. HPLC grade.
4.3 ethyl acetate.
4.4 n-hexane.
4.5 HLB solid phase extraction column. 60mg/3mL, or equivalent person.
4.6 5% methanol aqueous solution. Methanol 5mL, dissolved and diluted to 100mL with water.
4.7 0.05mol/L ammonium acetate solution. Take 3.15 g of ammonium acetate, dissolved and diluted to 1000mL with water, membrane filtration.
4.8 1mg/mL acetaminophen standard stock solution. Weigh accurately acetaminophen 10mg, in 10mL volumetric flask, dissolved with methanol
Solution and dilute to volume, formulated at a concentration of 1mg/mL of acetaminophen standard stock solution. -20 ℃ the following, valid for
3 months.
4.9 10μg/mL working solution of paracetamol standard. precise amount of 1mg/mL acetaminophen standard stock solution 1.0mL, in
100mL flask, dissolved in mobile phase and dilute to volume, formulated at a concentration of 10μg/working fluid acetaminophen standard mL.
Now with the current.
5. Apparatus
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 freezing high-speed centrifuge.
5.5 homogenizer.
5.6 vortex mixer.
5.7 circulating water pump.
5.8 stoppered centrifuge tube. 50mL.
5.9 filter. 0.45μm.
Preparation and Storage of sample 6
6.1 Preparation of the sample
Fresh or frozen blank or test tissue, fascia removed, 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 extract
Sample Weigh 5g ± 0.05g, centrifuge tube with stopper, ethyl acetate was added 20mL vortex 2min, 6000r/min centrifugal 15min,
The supernatant, in another centrifuge tube, the residue was added ethyl acetate 10mL, extraction was repeated once, the two supernatants were combined, 6000r/min from
Heart 10min, the supernatant was evaporated to dryness in a water bath 45 ℃, the residue was dissolved 3mL methanol, n-hexane was added 5mL, mixed, allowed to stand points
Layer, hexane layer was discarded, the lower layer was taken, dried with nitrogen at 45 ℃ water bath, dissolve the residue was washed with water 6mL, 10000r/min centrifugal 10min,
The supernatant was set aside.
7.2 Purification
HLB column eluted sequentially with methanol and 3mL 3mL water activation, taking stock solution through the column, controlling the flow rate of less than 2mL/min. 3mL water
5% methanol and 3mL rinse, 4 mL methanol, the eluate was collected, dried at 40 ℃ ~ 45 ℃ water bath nitrogen gas, the mobile phase 1.0mL
The residue was dissolved, 10000r/min centrifuge 5min, the supernatant for HPLC.
7.3 Preparation of standard curve
The precise amount of 10μg/mL working solution of paracetamol standard amount, diluted with mobile phase, concentration of formulated 10,25,50,100,
200,400,800 and 1600μg/L of the series of standard solution for HPLC assay. Peak area was measured to the vertical axis, corresponding to the standard
Standard solution concentration as the abscissa, the standard curve. Seeking regression equation and correlation coefficient.
7.4 Determination
7.4.1 LC Conditions
7.4.1.1 Column. C18 (250mm × 4.6mm, particle size 5μm), or equivalent person.
7.4.1.2 Mobile phase. methanol 0.05mol/L ammonium acetate solution (20 80, volume ratio).
7.4.1.3 flow rate. 1.0mL/min.
7.4.1.4 UV detection wavelength. 250nm.
7.4.1.5 Injection volume. 50μL.
7.4.1.6 Column temperature. 30 ℃.
7.4.2 Assay
Take a sample solution and standard solutions corresponding, for single or multi-point calibration, external standard method with peak area calculations. Standard solution and sample solution
Acetaminophen in response shall be within the linear range of the detection instrument. In the chromatographic conditions, sample was added standard solution and blank
HPLC chromatogram of solution are given in Appendix A.
7.5 Blank test
But without addition of the sample, the same steps employed in parallel operation.
8 and the result of the calculation expression
In a sample of the residual amount of acetaminophen drug according to formula (1).
X = A × cS × VAS × m
(1)
Where.
--- for X-residue amount of the phenol compound to try drugs acetylamino micrograms per kilogram (μg/kg);
A --- sample solution acetaminophen peak area;
cS --- standard working solution concentration of acetaminophen in micrograms per liter (μg/L);
V --- The residue was dissolved in mobile phase volume in milliliters (mL);
--- the AS standard working solution acetaminophen peak area;
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 sensitivity detection method, accuracy and precision
9.1 Sensitivity
The detection limit of the method of 3μg/kg, the limit of quantitation of 10μg/kg.
9.2 Accuracy
This method of adding 10μg/kg ~ 100μg/kg on recovery levels of 70% to 110%.
9.3 Precision
≤15% relative standard deviation in this method and inter - batch relative standard deviation of ≤15%.
Appendix A
Chromatogram
Figure A.1 acetaminophen chromatogram of the standard solution (10μg/L)
Figure A.2 in pig muscle blank sample chromatogram
Figure A.3 white pig muscle Add acetaminophen sample chromatogram (10μg/kg)
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