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GB 29684-2013: Determination of Erythromycin residues in aquatic products by Liquid Chromatography-tandem Mass Spectrometric method
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Determination of Erythromycin residues in aquatic products by Liquid Chromatography-tandem Mass Spectrometric method
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GB 29684-2013
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Basic data | Standard ID | GB 29684-2013 (GB29684-2013) | | Description (Translated English) | Determination of Erythromycin residues in aquatic products 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 | 11,184 | | Quoted Standard | GB/T 6682; GB/T 1.1-2000; SC/T 3016 | | Adopted Standard | GB/T 6682; GB/T 1.1-2000; SC/T 3016 | | 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 Aquatic Erythromycin residue detection sample preparation, liquid chromatography tandem mass spectrometry. This standard applies to fish Erythromycin residue testing. | GB 29684-2013: Determination of Erythromycin residues in aquatic products by Liquid Chromatography-tandem Mass Spectrometric method
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Determination of Erythromycin residues in aquatic products by Liquid Chromatography-tandem Mass Spectrometric method
National Standards of People's Republic of China
National Food Safety Standard
Determination of the residues in aquatic erythromycin
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 the residues in aquatic erythromycin
Liquid chromatography - tandem mass spectrometry
1 Scope
This standard specifies the aquatic Erythromycin Residues sample preparation and liquid chromatography - tandem mass spectrometry.
This standard applies to edible fish tissues detecting the residual amount of erythromycin.
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
SC/T 3016 aquatic sampling
Principle 3
Erythromycin remaining in a sample, extracted with acetonitrile, hexane degreasing, an HLB column purified liquid chromatography - tandem mass spectrometry, internal standard method
Quantitative.
4 Reagents and materials
The following reagents used, unless otherwise stated were of analytical reagent; water as a water line with GB/T 6682 provisions.
4.1 erythromycin Standard. Content ≥97%.
Erythromycin 4.2 isotope internal standard standard. erythromycin isotope (erythromycinA, N, N-Dimethyl-13C2) content of ≥90%.
4.3 Acetonitrile. chromatographically pure.
4.4 hexane. chromatography.
4.5 Methanol. HPLC grade.
4.6 acetic acid.
4.7 sodium chloride.
4.8 twelve disodium hydrogen phosphate water.
4.9 phosphoric acid.
4.10 HLB solid phase extraction column.200mg/6mL, or equivalent person.
4.11 0.1mol/L phosphate buffer. Take 17.92 g disodium hydrogen phosphate dodecahydrate, dissolve and dilute to 500mL with water, adjusted with phosphoric acid
pH to 8.0, now with the current.
4.12 40% methanol solution. Methanol 40mL, dissolved and diluted to 100mL with water.
4.13 30% methanol solution. Methanol 30mL, dissolved and diluted to 100mL with water.
4.14 0.01 ‰ acetic acid aqueous solution. Take 10μL of acetic acid, dissolved and diluted with water to 1000mL.
4.15 100μg/mL standard stock solution of erythromycin. erythromycin standard accurately weighed 10mg, in 100mL flask, dissolved in methanol and
Diluted to the mark, formulated at a concentration of 100μg/mL standard stock solution of erythromycin. The following -18 ℃ dark preservation, valid for six months.
4.16 5μg/mL erythromycin standard working solution. precise amount of 100μg/mL standard stock solution of erythromycin 500μL, in 10mL volumetric flask
, Diluted with methanol to scale, formulated at a concentration of working standard solution of erythromycin 5μg/mL of. The following -18 ℃ dark preservation, valid
3 months.
4.17 100μg/mL erythromycin isotope internal standard standard stock solution. Weigh accurately erythromycin isotope internal standard standard 10mg, in
100mL flask, dissolved in methanol and diluted to the mark, formulated at a concentration of 100μg/mL erythromycin isotope internal standard stock standard
liquid. The following -18 ℃ dark preservation, valid for six months.
4.18 200ng/mL erythromycin isotope internal standard working standard solution. precise amount of 100μg/mL standard erythromycin isotope internal standard reservoir
200 L was prepared, in 100mL volumetric flask, dilute to the mark with methanol, formulated at a concentration of 200ng/mL in the standard isotope erythromycin
Standard working solution. The following -18 ℃ dark preservation, valid for three months.
5. Apparatus
5.1 liquid chromatography - tandem mass spectrometry. ion source distribution.
5.2 Analytical balance. a sense of volume 0.00001g.
5.3 Balance. a sense of the amount of 0.01g.
5.4 oscillator.
5.5 homogenizer.
5.6 centrifuge.
5.7 pH meter.
5.8 rotary evaporator.
5.9 eggplant-shaped flask. 100mL.
5.10 centrifuge tube. 50mL.
5.11 filter. 0.22μm.
Preparation and Storage of sample 6
6.1 Preparation of the sample
Product water test blank or edible 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
-20 ℃ below Save to 3 months.
Determination Step 7
7.1 extract
Sample Weigh 5g ± 0.05g, in 50mL centrifuge tube, was added 200ng/mL erythromycin isotope internal standard working standard solution 50 L,
Acetonitrile was added 15mL, immediately dispersed with stirring, ultrasonic 5min, shaking 5min, 4000r/min centrifugal 10min, supernatant, the other
Centrifuge tube, the residue was added acetonitrile 5mL, extraction was repeated once, the two supernatants were combined, and sodium chloride in hexane 2g 15mL, shaking
5min, 4000r/min centrifugal 10min, the upper n-hexane solution was discarded, the lower layer was taken, in 100mL eggplant-shaped flask, to rotary evaporation at 40 ℃
Dry with phosphate buffer solution 5mL, dissolve the residue, hexane was added 5mL, mixing 1min, transferred to centrifuge tubes, 6000r/min centrifugal
5min, n-hexane layer was discarded, together with n-hexane 5mL, the operation is repeated once, and the lower layer was set aside.
7.2 Purification
5mL HLB column successively with methanol, water, phosphate buffered saline 5mL and 5mL activated, taking stock solution through the column with phosphate buffer
Washed with 5mL centrifuge tube, the washing solution through the column, the stream of dry, washed with water 5mL methanol and 5mL of 40% was rinsed, drained, washed with methanol 8mL
, Collecting eluate, in the eggplant-shaped flask, at 40 ℃ rotary evaporation to dryness, with 30% 1.0mL residue was dissolved in methanol, filter through
Filter for liquid chromatography - tandem mass spectrometry.
7.3 Preparation of standard curve
The precise amount of 5μg/mL erythromycin standard working solution and 200ng/mL erythromycin isotope internal standard working standard solution amount, with
30% methanol solution and dissolving and diluting the standard Erythromycin isotopic concentration of 10ng/mL and the concentration of erythromycin 1,5,10,
25, 50 and 500ng/mL standard solution series for liquid chromatography - tandem mass spectrometry. A characteristic mass ion peak area
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 × 2.1mm, particle size 5μm), or equivalent person.
7.4.1.2 Mobile phase. A. methanol, B. 0.01 ‰ aqueous acetic acid.
7.4.1.3 gradient elution. 0.0min ~ 1.0min, 30% A; 1.01min ~ 7min, 95% A; 7.01min ~ 17min; 30% A.
7.4.1.4 flow rate. 0.3mL/min.
7.4.1.5 Column temperature. 25 ℃.
7.4.1.6 Injection volume. 25μL.
7.4.2 MS conditions
7.4.2.1 ion source. electrospray ionization source.
7.4.2.2 Scan mode. positive ion scan.
7.4.2.3 Detection mode. multiple reaction monitoring.
7.4.2.4 Spray voltage. 4700V.
7.4.2.5 ion transfer capillary temperature. 300 ℃.
The collision-induced dissociation voltage source 7.4.2.6. 8V.
7.4.2.7 atomizing gas flow rate. 12.3L/h.
7.4.2.8 auxiliary gas flow rate. 1.7L/h.
7.4.2.9 qualitative, quantitative and collision energy of ions shown in Table 1.
Table 1 Qualitative and quantitative and collision energy of ions
The target compound
Qualitative ion pair
m/z
Quantitative ion pair
m/z
Collision energy
eV
Erythromycin 734.4 > 157.9
734.4 > 576.0
734.4 > 157.9
Erythromycin parity
Internal standard prime 736.5 > 159.9 736.5 > 159.9 30
7.4.3 Assay
7.4.3.1 qualitative determination
By retention time of sample chromatogram with retention times corresponding to the standard, characteristic peaks corresponding to the ion concentration of the standard color
Characterized in contrast to qualitative ion peaks. Sample and standard deviation of the relative retention time of not more than 5%; relative abundance of ions in a sample wherein
Consistent with the relative abundance of a considerable concentration of the standard solution, the relative abundance of the deviation does not exceed ± 20%, may be present in the sample is determined corresponding
Was measured.
7.4.3.2 quantitative determination
Take a sample and standard solutions, by external standard method, in order to quantify the peak area, the standard solution and sample solution erythromycin response value should be at
The linear range of the detection equipment. In the above-described chromatography - mass spectrometry under conditions erythromycin standard solution added in the blank and wherein a sample solution ion mass
Amount chromatogram 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
Erythromycin residues in a sample according to formula (1).
X =
c × V
(1)
Where.
--- for the residual amount of X-try erythromycin compound in micrograms per kilogram (μg/kg);
C --- erythromycin sample solution concentration unit nanograms per milliliter (ng/mL);
The residue was dissolved --- V the volume in milliliters (mL);
m --- try supply feed mass in grams (g).
Note. The blank value should be subtracted from the calculation results. Results are expressed as the arithmetic mean of the two 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 ~ 400μg/kg on recovery levels of 70% to 120%.
9.3 Precision
The relative standard deviation of the method ≤15%, inter-assay relative standard deviation ≤15%.
Appendix A
The ion mass chromatogram
Description.
1 --- erythromycin wherein ion mass chromatogram (734.4 > 575.9);
2 --- erythromycin wherein ion mass chromatogram (734.4 > 159.9);
3 --- erythromycin isotopic ion mass chromatogram characteristic (736.50 > 159.9).
Figure A.1 erythromycin Erythromycin isotope standard and standard solution wherein ion mass chromatogram (25ng/mL)
Description.
1 --- erythromycin wherein ion mass chromatogram (734.4 > 575.9);
2 --- erythromycin wherein ion mass chromatogram (734.4 > 159.9);
3 --- erythromycin isotopic ion mass chromatogram characteristic (736.50 > 159.9).
Figure A.2 Grass edible tissue sample blank wherein the ion mass chromatogram
Description.
1 --- erythromycin wherein ion mass chromatogram (734.4 > 575.9);
2 --- erythromycin wherein ion mass chromatogram (734.4 > 159.9);
3 --- erythromycin isotopic ion mass chromatogram characteristic (736.50 > 159.9).
Figure A.3 Grass edible tissue sample blank add features erythromycin ion mass chromatogram (5μg/kg)
3102-
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