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GB 29686-2013: Determination of Avilamycin residues in edible tissues of swine by Liquid Chromatography-tandem Mass Spectrometric method
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Determination of Avilamycin residues in edible tissues of swine by Liquid Chromatography-tandem Mass Spectrometric method
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GB 29686-2013
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Basic data
| Standard ID | GB 29686-2013 (GB29686-2013) |
| Description (Translated English) | Determination of Avilamycin residues in edible tissues of swine by Liquid Chromatography-tandem Mass Spectrometric method |
| Sector / Industry | National Standard |
| Classification of Chinese Standard | C53 |
| Classification of International Standard | 67.020 |
| Word Count Estimation | 11,118 |
| 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 pig edible tissues Avilamycin residue detection sample preparation, liquid chromatography tandem mass spectrometry. This standard applies to pig muscles the detection of drug residues. |
GB 29686-2013: Determination of Avilamycin residues in edible tissues of swine by Liquid Chromatography-tandem Mass Spectrometric method
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Determination of Avilamycin residues in edible tissues of swine by Liquid Chromatography-tandem Mass Spectrometric method
National Standards of People's Republic of China
National Food Safety Standard
Determination of Residues avilamycin edible tissues of pigs
Liquid chromatography - tandem 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 Residues avilamycin edible tissues of pigs
Liquid chromatography - tandem mass spectrometry
1 Scope
This standard specifies the edible tissues of porcine avilamycin Residues sample preparation and liquid chromatography - tandem mass spectrometry.
This standard applies to porcine muscle, fat/skin, liver and kidney detecting residual amounts of avilamycin.
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
Avilamycin remaining in a sample, extracted with acetone and hydrolyzed with sodium hydroxide solution, extracted with ethyl acetate, alumina SPE
Purification to dicamba as internal standard, liquid chromatography - tandem mass spectrometry APCI measured internal standard.
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 avilamycin, avilamycin residue standard marker DIA. content ≥98%.
4.2 Internal standard. dicamba standard. content ≥98%.
4.3 Methanol. HPLC grade.
4.4 n-hexane.
4.5 Acetonitrile. chromatographically pure.
4.6 ethyl acetate.
4.7 acetone.
4.8 formic acid.
4.9 sodium hydroxide.
4.10 phosphate.
4.11 SPE column of neutral alumina. 1000mg/6mL, or equivalent person.
4.12 1mol/L sodium hydroxide solution. take sodium hydroxide 4g, dissolve and dilute to 100mL with water.
4.13 Eluent. Take acid 5mL, dissolved in acetonitrile and diluted to 100mL.
4.14 1mg/mL and avilamycin avilamycin marker residue DIA standard stock solution. accurately weighed and Avila avilamycin
DIA each marker neomycin residue 10mg, respectively 10mL volumetric flask, dissolved in methanol and diluted to the mark, formulated at a concentration of 1mg/mL
The residue avilamycin and avilamycin marker DIA standard stock solution. 2 ℃ ~ 4 ℃ storage period of one month.
4.15 10μg/mL and the avilamycin avilamycin marker residue DIA standard working solution. precise amount of 1mg/mL mycophenolic Avila
Hormone and residual avilamycin was marked DIA 1.0mL each standard stock solution, respectively, 100mL flask, dissolved in methanol and diluted to
Scale, formulated at a concentration of 10μg/mL and the avilamycin avilamycin marker residue DIA working standard solution. 2 ℃ ~ 4 ℃
, Valid for one month.
4.16 1mg/mL internal standard dicamba standard stock solution. Weigh accurately dicamba 10mg, in 10mL flask,
Dissolved in methanol and diluted to volume, formulated at a concentration of 1mg/mL of dicamba stock standard solution. 2 ℃ ~ 4 ℃ stored, effective
1 month.
4.17 2μg/mL internal standard dicamba standard working solution. precise amount of 1mg/mL dicamba stock standard solution
200 L, in 100mL flask, dissolved in methanol and diluted to the mark, formulated at a concentration of 2μg/mL in the standard work dicamba
As a liquid. 2 ℃ ~ 4 ℃ storage period of one month.
5. Apparatus
5.1 High Performance Liquid Chromatography - Tandem Mass spectrometer. with atmospheric pressure chemical ionization source (APCI).
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 oscillator.
5.6 vortex mixer.
5.7 homogenizer.
5.8 Nitrogen blowing instrument.
5.9 rotary evaporator.
5.10 SPE.
5.11 round-bottomed flask. 50mL.
5.12 centrifuge tube. 15mL, 50mL.
Preparation and Storage of sample 6
6.1 Preparation of the sample
Fresh or frozen 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
Muscle or fat was weighed sample 2g ± 0.05g, liver or kidney sample 1g ± 0.05g, in 15mL centrifuge tube, and acetone
4 mL, vortexed 5min, at 6000r/min centrifugal 10min, supernatant at 50mL round bottom flask. The residue was added acetone 4mL,
The extraction was repeated twice, and the combined supernatant three times, at 60 deg.] C rotary evaporated to dryness, the residue was dissolved with 1mol/L sodium hydroxide solution, 4 mL,
Go 50mL centrifuge tube, at 70 deg.] C water bath for 2h, extracted with 85% phosphoric acid adjusted to pH 1.0, was added 4 mL of ethyl acetate, were mixed and
6000r/min centrifugal 10min, supernatant to another centrifuge tube, was repeated twice, and the combined supernatant three times, plus 2μg/mL dichloromethoxy
Benzoic acid 0.5 mL internal standard (except for the blank sample), the standby mix.
7.2 Purification
10mL ethyl acetate and extracted with an alumina column activated, taking stock solution passed through the column, 5mL each with n-hexane, ethyl acetate and methanol 5mL
5mL, and eluted twice with an eluent, 7 mL each, were collected eluent at 50 ℃ rotary evaporated to dryness, residue dissolved in methanol 1.0mL
It was vortexed for liquid chromatography - tandem mass spectrometry.
7.3 Preparation of standard curve
The precise amount of 10μg/mL avilamycin marker residue amount DIA working standard solution, diluted with methanol, formulated at a concentration of 5,
50,100,200,400 and 800μg/L standard solution series for liquid chromatography - tandem mass spectrometry. Ion mass peak characteristics to surface
Volume of the ordinate, the abscissa the concentration of the standard solution, the standard curve. Seeking regression equation and correlation coefficient.
7.4 Determination
7.4.1 LC Conditions
7.4.1.1 Column. C18 (150mm × 4.6mm, particle size 5μm), or equivalent person.
7.4.1.2 Mobile phase. methanol-water (50 50, volume ratio).
7.4.1.3 flow rate. 0.6mL/min.
7.4.1.4 Injection amount. 10μg/L.
7.4.1.5 Column temperature. 40 ℃.
7.4.2 MS conditions
7.4.2.1 ion source. APCI.
7.4.2.2 Scan mode. negative ion scan.
7.4.2.3 Detection mode. selective reaction monitoring.
7.4.2.4 evaporation temperature. 400 ℃.
7.4.2.5 Ion transfer tube temperature. 275 ℃.
7.4.2.6 Sheath Gas Pressure. 25arb.
7.4.2.7 Auxiliary gas pressure. 5arb.
7.4.2.8 selected reaction monitoring optimization parameters in Table 1.
Table 1 avilamycin selected reaction monitoring of optimization parameters
Drug Name
Relative retention time
min
Parent ion
Mass number
Qualitative and ion collision energy
eV
Quantitative ion and collision energy
eV
Avilamycin Residues
DIA marker
7.10 249 249 > 189 (23)
249 > 205 (16)
249 > 205 (16)
Dicamba 8.80 219 219 > 159 (18)
219 > 145 (15)
219 > 175 (8)
7.4.3 Assay
7.4.3.1 qualitative determination
By retention time of sample chromatogram with retention times of the respective standards, wherein each of the ion peaks and the corresponding concentration of the standard
Wherein each of the ion peaks qualitative contrast. Sample and standard deviation of the relative retention time of not more than 5%; with a sample wherein ions
Consistent with the abundance relative abundance fairly mixed standard solution concentration, relative abundance does not exceed a predetermined deviation Table 2, the sample can be stored is determined
The respective analyte.
The maximum allowable deviation relative ion abundance qualitative determination of Table 2%
The relative ion abundances > 50 20 ~ 50 10 ~ 20 ≤10
Permissible relative deviation ± 20 ± 25 ± 30 ± 50
Ratio for the sample and standard solutions try quantitative ion area of single-point calibration for quantification.
7.4.3.2 quantitative determination
Take a sample and standard solutions, the external standard method to avilamycin peak area, the standard solution and the sample solution response values are
It should be in the linear range of the detection instrument. In the above-described chromatography - mass spectrometry under conditions avilamycin added standard solution and the blank sample solution Laid
Intrinsic ion mass chromatogram given 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
Residues in the specimens avilamycin marker residue (DIA) according to formula (1).
X =
A × cS × ci × ASi × V
AS × cSi × Ai × m
(1)
Where.
--- for the residual amount of X-try DIA compound, in units of micrograms per kilogram (μg/kg);
A --- The sample solution DIA peak area;
Standard solution concentration cS --- DIA, expressed in nanograms per milliliter (ng/mL);
--- CI concentration in the sample solution in the standard units of nanograms per milliliter (ng/mL);
Peak area of the internal standard solution ASi --- standard substance;
V --- the final volume of the sample solution, in milliliters (mL);
--- the AS standard solution of DIA peak area;
Concentration of a standard solution of cSi --- standard material, in units of nanograms per milliliter (ng/mL);
Peak area of the internal standard in the sample solution --- AI thereof;
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
This limit of detection in muscle and adipose tissue was 10μg/kg, the limit of quantitation of 20μg/kg; subject in liver and kidney tissues
LOD was 20μg/kg, the limit of quantitation of 50μg/kg.
9.2 Accuracy
This method of adding 20μg/kg ~ 600μg/kg on recovery levels of 70% to 120%.
9.3 Precision
The relative standard deviation of the method ≤20%, inter-assay relative standard deviation ≤20%.
Appendix A
The ion mass chromatogram
Figure A.1 standard solution wherein ion mass chromatogram (DIA5μg/L, dicamba 1μg/mL)
Figure A.2 characterized in porcine kidney blank sample ion mass chromatogram
Figure A.3 pig kidney sample blank add avilamycin wherein ion mass chromatogram (50μg/kg)
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