Path:
Home >
GB >
Page142 > GB 29709-2013
Home >
Standard_List >
GB >
Page142 > GB 29709-2013
US$209.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email.
GB 29709-2013: Determination of Azaperone and metabolite in animal derived food by High Performance Liquid Chromatographic method
Status: Valid
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| GB 29709-2013 | English | 209 |
Add to Cart
|
3 days [Need to translate]
|
Determination of Azaperone and metabolite in animal derived food by High Performance Liquid Chromatographic method
| Valid |
GB 29709-2013
|
PDF similar to GB 29709-2013
Basic data
| Standard ID | GB 29709-2013 (GB29709-2013) |
| Description (Translated English) | Determination of Azaperone and metabolite 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 | 9,976 |
| 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 azapirone, piperazine nitrogen metabolites alcohol residue detection sample preparation, high-performance liquid chromatographic method. |
GB 29709-2013: Determination of Azaperone and metabolite in animal derived food 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 Azaperone and metabolite in animal derived food by High Performance Liquid Chromatographic method
National Standards of People's Republic of China
National Food Safety Standard
Animal foods and metabolite azapirone
Residues in HPLC
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 and metabolite azapirone
Residues in HPLC
1 Scope
This standard specifies the sample preparation and high performance liquid chromatographic method in animal food azapirone of nitrogen and residual piperidine alcohol metabolite detected.
This standard applies to porcine muscle, sebum, liver and kidney tissues and the detection of residual amount of azapirone nitrogen piperidin alcohol metabolites.
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.
Specifications and test methods for laboratory water GB/T 6682 analysis.
Principle 3
In a sample and the residual azapirone metabolite, extracted with acetonitrile, hexane degreasing, MCX column purification, HPLC, external standard
The statutory amount.
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 azapirone, piperazine nitrogen alcohols standard. content ≥98%.
4.2 Acetonitrile. chromatographically pure.
4.3 n-hexane.
4.4 concentrated ammonia.
4.5 methanol.
4.6 ammonium acetate.
4.7 formic acid.
4.8 MCX SPE. 60mg/3mL, or equivalent person.
4.9 2% aqueous formic acid. formic acid take 2mL, dissolve and dilute to 100mL with water.
4.10 5% ammoniated methanol. aqueous ammonia Take 5mL, dissolved in methanol and diluted to 100mL.
4.11 5mmol/L ammonium acetate solution. Take ammonium acetate 0.385g, dissolved in water and diluted to 1000mL, membrane filtration.
4.12 1mg/mL standard stock solution. Weigh accurately azapirone piperazine nitrogen and alcohol in each standard 10mg, respectively 10mL volumetric flask, washed with methanol
Dissolved and diluted to the mark, dubbed the concentration of the standard stock solution 1mg/mL of. The following -20 ℃ dark preservation, valid for three months.
4.13 1μg/mL working standard solutions. precise amount of each 1mg/mL standard stock solution azapirone piperidine nitrogen and the alcohol of each stock standard solution
0.1 mL, to 100mL volumetric flask, dilute to volume with methanol to prepare a working standard solutions at a concentration of 1μg/mL of. At -20 ℃
Stored in the dark period of three months.
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 nitrogen blow device.
5.6 vortex mixer.
5.7 SPE.
5.8 ultrasonic cleaning machine.
5.9 homogenizer.
5.10 centrifuge tube.
5.11 filter. 0.22μm.
Preparation and Storage of sample 6
6.1 Preparation of the sample
Fresh or frozen tissue white, the 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, a centrifuge tube, acetonitrile was added 10mL, vortexed 1min, ultrasonic 2min, 5000r/min centrifugal
5min, the supernatant, the residue was added 10mL of acetonitrile extraction was repeated once, the two supernatants were combined. 40 ℃ rotary evaporated to dryness in a water bath. use
2% formic acid were dissolved 5mL aqueous residue was added 4 mL of n-hexane, mixed, 5000r/min centrifugal 5min, n-hexane layer was discarded, the standby.
7.2 Purification
MCX cartridge 3mL successively with methanol, water and 2% aqueous formic acid 3mL 3mL activation, taking stock solution through the column, the flow rate is less than the control
1mL/min, with 2% aqueous formic acid and methanol 3mL 3mL rinsed, drained, washed with 5% ammoniated methanol 4mL. The eluent was collected in
40 ℃ nitrogen blow, the residue was dissolved in mobile phase was 1.0mL, Vortex for HPLC.
7.3 Preparation of standard curve
The precise amount of 1μg/mL working standard solutions amount, diluted with methanol, and formulated to a concentration of 10,20,50,100,200,500
1000μg/L mixed standard solution series. Each concentration was repeated 3 times for HPLC, to measure the average peak area obtained for the vertical
Coordinates, the corresponding standard concentration as the abscissa, the standard curve. Seeking regression equation and correlation coefficient.
7.4 Determination
7.4.1 Chromatographic conditions
7.4.1.1 Column. C18 (250mm × 4.6mm, particle size 5μm), or equivalent person.
7.4.1.2 mobile phase. acetonitrile 5mmol/L ammonium acetate solution (50 50, volume ratio).
7.4.1.3 flow rate. 1mL/min.
7.4.1.4 UV detection wavelength. 250nm.
7.4.1.5 Column temperature. 40 ℃.
7.4.1.6 Injection volume. 50μL.
7.4.2 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
Azapirone and liquid nitrogen piperidin alcohols response value should be within the linear range of the detection instrument. In the chromatographic conditions, the standard solution and blank add
HPLC chromatograms of the sample solution in Appendix A.
7.5 Blank test
But without addition of the sample, the same steps employed in parallel operation.
Calculation and Expression of Results 8
The specimens azapirone alcohol residues and piperazine nitrogen (μg/kg) according to formula (1) to (3) Calculated.
Single-point calibration.
c =
cSA
AS
(1)
Calibration or standard curve by. AS = acS b to obtain a and b, then
c =
Ab
(2)
X =
cV
(3)
Where.
C --- try to supply feed concentration in the solution and the appropriate azapirone metabolite, in micrograms per liter (μg/L);
cS --- standard working solution in a concentration corresponding azapirone and metabolites, in micrograms per liter (μg/L);
A --- area of the respective sample azapirone and metabolite peaks;
--- the AS standard working solution in the corresponding area of the azapirone and metabolite peaks;
--- for X-try respective feed azapirone and metabolite residues micrograms per kilogram (μg/kg);
V --- The residue was dissolved in mobile phase 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 2μg/kg, the limit of quantitation of 5μg/kg.
9.2 Accuracy
This method in the muscle, tissue sebum 5μg/kg ~ 60μg/kg, liver and kidney tissues at 5μg/kg ~ 100μg/kg addition concentration
On recovery levels of 60% to 110%.
9.3 Precision
≤20% relative standard deviation in this method and inter - batch relative standard deviation of ≤20%.
Appendix A
Chromatogram
Figure A.1 azapirone and metabolite standards solution chromatogram (10μg/L)
Figure A.2 in pig muscle blank sample chromatogram
Figure A.3 in pig muscle and blank add azapirone metabolite sample chromatogram (5μg/kg)
Tips & Frequently Asked Questions:
Question 1: How long will the true-PDF of GB 29709-2013_English be delivered?
Answer: Upon your order, we will start to translate GB 29709-2013_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. The lengthier the document the longer the lead time.
Question 2: Can I share the purchased PDF of GB 29709-2013_English with my colleagues?
Answer: Yes. The purchased PDF of GB 29709-2013_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet.
Question 3: Does the price include tax/VAT?
Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs):
List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?
Answer: Yes. If you need your currency to be printed on the invoice, please write an email to
[email protected]. In 2 working-hours, we will create a special link for you to pay in any currencies. Otherwise, follow the normal steps: Add to Cart -- Checkout -- Select your currency to pay.