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GB 29697-2013: Determination of Diazepam and Methaqualone residues in animal derived food by Gas Chromatography-Mass Spectrometric method
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Determination of Diazepam and Methaqualone residues in animal derived food by Gas Chromatography-Mass Spectrometric method
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GB 29697-2013
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Basic data
| Standard ID | GB 29697-2013 (GB29697-2013) |
| Description (Translated English) | Determination of Diazepam and Methaqualone 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 | 10,156 |
| 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 diazepam, methaqualone residue detection sample preparation, gas chromatography mass spectrometry. |
GB 29697-2013: Determination of Diazepam and Methaqualone residues in animal derived food by Gas Chromatography-Mass Spectrometric method
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Determination of Diazepam and Methaqualone residues in animal derived food by Gas Chromatography-Mass Spectrometric method
National Standards of People's Republic of China
National Food Safety Standard
Animal foods methaqualone and diazepam multi-residue
By 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
Animal foods methaqualone and diazepam multi-residue
By gas chromatography - mass spectrometry
1 Scope
This standard specifies the sample preparation and gas chromatography of animal foods and diazepam methaqualone of Residues - mass spectrometry.
This standard applies to pigs diazepam and methaqualone residues detected in muscle tissue.
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 diazepam and methaqualone, extracted with acetonitrile, hexane degreasing, C18 column purification, gas chromatography - mass spectrometry, external standard method
Quantitative.
4 Reagents and materials
The following reagents used, unless otherwise stated are analytical reagents, water as a water line with GB/T 6682 provisions.
4.1 diazepam, methaqualone reference. content ≥99.5%.
4.2 Acetonitrile. chromatographically pure.
4.3 hexane. chromatography.
4.4 Methanol. HPLC grade.
4.5 toluene. chromatography.
4.6 C18 solid phase extraction column. 500mg/3mL, or equivalent person.
4.7 50% aqueous methanol. Methanol 50mL, dissolved and diluted to 100mL with water.
4.8 70% aqueous methanol. Methanol 70mL, dissolved and diluted to 100mL with water.
4.9 200μg/mL methaqualone and diazepam standard stock solution. Precision Weigh methaqualone and diazepam each standard 10mg, respectively,
50mL volumetric flask, dissolved in methanol and diluted to the mark, formulated at a concentration of 200μg/mL methaqualone and diazepam standard stock solution.
-20 ℃ below, valid for six months.
4.10 50μg/mL standard stock solution mixed. precise amount of 200μg/mL standard stock solution diazepam and 200μg/mL standard methaqualone
Each stock solution 25mL, in 100mL volumetric flask, dilute to volume with methanol, formulated at a concentration of 50μg/mL standard stock solution mixed.
-20 ℃ below, valid for six months.
4.11 10μg/mL standard stock solution mixed. precise amount of 50μg/mL standard stock solution mixed 10mL, 50mL in the flask, A
Alcohol diluted to the mark to prepare a mixed standard stock solution at a concentration of 10μg/mL of. -20 ℃ below, valid for six months.
5. Apparatus
5.1 Gas chromatography - mass spectrometry. with electron impact ionization (EI).
5.2 Analytical balance. a sense of the amount of 0.00001g.
5.3 Balance. a sense of the amount of 0.01g.
5.4 a vortex.
5.5 centrifuge.
5.6 homogenizer.
5.7 rotary evaporator.
5.8 Nitrogen blowing instrument.
5.9 SPE.
5.10 ultrasonic cleaner.
5.11 heart-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 extract
Sample Weigh 2g ± 0.02g, a centrifuge tube, acetonitrile was added 20mL, ultrasonic water bath for 5min. 4000r/min centrifugal 10min, the
The supernatant in the heart-shaped flask. At 50 deg.] C and rotary evaporated to near 5mL, 7.5 mL of n-hexane was added, mixing was allowed to stand, the supernatant was discarded. Take the lower liquid at
50 ℃ nitrogen purge to 1mL, water was added 4mL, mixing spare.
7.2 Purification
C18 column successively with methanol and 3mL 3mL water activation, taking stock solution through the column, washed with 50% aqueous methanol with 3mL, 70% A
3mL aqueous alcohol solution, collecting eluate, blown dry with nitrogen at 50 ℃, the residue was dissolved with 200μL of acetonitrile, gas chromatography - mass spectrometry
Determination.
7.3 Preparation of standard curve
The precise amount of 10μg/mL working standard solutions amount, diluted with methanol, and formulated to a concentration of 1,10,50,100,500
1000ng/mL standard solution series, gas chromatography - mass spectrometry. Peak area was measured to the vertical axis, the corresponding concentration of the standard solution
Degree abscissa, the standard curve. Seeking regression equation and correlation coefficient.
7.4 Determination
7.4.1 Reference Gas chromatography conditions
7.4.1.1 Gas Chromatographic Column. DB-5MS column (30m × 0.25mm, diameter 0.25μm), or equivalent person.
7.4.1.2 Carrier gas. helium.
7.4.1.3 Carrier gas flow rate. 0.9mL/min.
7.4.1.4 Inlet temperature. 290 ℃.
7.4.1.5 Column temperature. initial temperature 150 ℃, holding 1min, 10 ℃/min temperature programmed to 290 ℃, maintained 4min.
7.4.1.6 Injection volume. 1μL, constant current mode splitless.
7.4.2 Mass Reference Conditions
7.4.2.1 electron impact ionization (EI).
7.4.2.2 electron impact energy. 70eV.
7.4.2.3 Ion source temperature. 230 ℃.
7.4.2.4 Quadrupole temperature. 150 ℃.
7.4.2.5 Solvent delay. 9min.
7.4.2.6 Detection Mode. selected ion detection.
7.4.2.7 qualifier ion. diazepam of m/z283, m/z256, m/z241, m/z221; methaqualone of m/z250, m/z235, m/z217,
m/z91.
7.4.2.8 quantitatively ion. diazepam of m/z256; methaqualone of m/z235.
7.4.3 Assay
7.4.3.1 qualitative determination
The drug content in the sample solution, the volume of selected peak area close to the standard working solution and the like injections of the sample solution and the like. By air
Relative retention time and MS-SIM common characterization. Retention time of the sample solution and standard pharmaceutical test substance relative deviation is not
1%, and the difference in the relative abundance of the selected ion which is less than 20%. Standard solution of diazepam and methaqualone, blank and blank samples
Selected ion chromatogram of the sample is added in Appendix A.
7.4.3.2 quantitative determination
Working standard solutions were taken and the corresponding amount of the sample solution concentration, single-point calibration for multi-point calibration, chromatographic peak area. standard
And diazepam solution and sample solution methaqualone response value should be in the linear range of the detection instrument, sample solution injection process parameters should be inserted
Standard working solution.
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
Try feed for diazepam and methaqualone residues according to formula (1).
X =
Ai × cS × 5 × V
AS × m
(1)
Where.
--- for the respective X-diazepam try and feed residues methaqualone, micrograms per kilogram (μg/kg);
AI --- respective sample solution methaqualone and diazepam peak area;
--- the AS standard solution diazepam respective peak area and methaqualone;
cS --- respective methaqualone and diazepam concentration, in units of nanograms per milliliter (ng/mL) in standard solution;
V --- volume of the sample solution, 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 0.5μg/kg, the limit of quantitation was 1μg/kg.
9.2 Accuracy
This method of adding 1μg/kg ~ 50μg/kg on recovery levels of 70% to 120%.
9.3 Precision
The relative standard deviation of the method ≤15%, inter-assay relative standard deviation ≤20%.
Appendix A
Chromatogram
Figure A.1 methaqualone and diazepam selected ion chromatogram of the standard solution (10μg/L)
Figure A.2 in pig muscle selected ion chromatogram of blank sample
Figure A.3 is added in pig muscle blank diazepam, methaqualone selected ion chromatogram of the sample (1μg/kg)
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