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GB 31658.24-2022: (National food safety standards-Determination of seduromycin residues in animal foods by liquid chromatography-tandem mass spectrometry)
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(National food safety standards-Determination of seduromycin residues in animal foods by liquid chromatography-tandem mass spectrometry)
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GB 31658.24-2022
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Basic data | Standard ID | GB 31658.24-2022 (GB31658.24-2022) | | Description (Translated English) | (National food safety standards-Determination of seduromycin residues in animal foods by liquid chromatography-tandem mass spectrometry) | | Sector / Industry | National Standard | | Classification of Chinese Standard | X04 | | Word Count Estimation | 10,164 | | Date of Issue | 2022-09-20 | | Date of Implementation | 2023-02-01 | | Issuing agency(ies) | National Health Commission of the People's Republic of China, State Administration for Market Regulation | GB 31658.24-2022: (National food safety standards-Determination of seduromycin residues in animal foods by liquid chromatography-tandem mass spectrometry)
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National Health Commission of the People's Republic of China
National Food Safety Standards
Determination of seduromycin residues in food of animal origin
Liquid Chromatography-Tandem Mass Spectrometry
National Standards of People's Republic of China
release
State Administration for Market Regulation
Ministry of Agriculture and Rural Affairs of the People's Republic of China
foreword
This document is in accordance with the provisions of GB/T 1.1-2020 "Guidelines for Standardization Work Part 1.Structure and Drafting Rules for Standardization Documents"
drafting.
This document is published for the first time.
National Food Safety Standards
Determination of seduromycin residues in food of animal origin
Liquid chromatography-tandem mass spectrometry
1 Scope
This document specifies the ultra-high performance liquid chromatography-tandem mass spectrometry method for the determination of seduromycin in food of animal origin.
This document is applicable to the determination of sedumecin residues in chicken muscle and liver tissue.
2 Normative references
The content in the following documents constitutes the essential provisions of this document through normative references in the text. Among them, the dated reference documents,
Only the version corresponding to the date applies to this document; for undated references, the latest version (including all amendments) applies to this document
document.
GB/T 6682 Analytical laboratory water specifications and test methods
3 Terms and Definitions
This document does not have terms and definitions that need to be defined.
4 principles
The residual seduramycin in the sample was extracted with acetonitrile, purified by solid-phase extraction column, detected by ultra-high performance liquid chromatography-tandem mass spectrometry, and external standard method.
Quantitative.
5 Reagents and materials
Unless otherwise specified, all reagents are of analytical grade; water is grade-1 water in accordance with GB/T 6682.
5.1 Reagents
5.1.1 Acetonitrile (CH3CN). chromatographically pure.
5.1.2 Methanol (CH3OH). chromatographically pure.
5.1.3 Formic acid (HCOOH). chromatographically pure.
5.1.4 Dichloromethane (CH2Cl2).
5.2 Solution preparation
5.2.1 50% acetonitrile solution. take 50mL of acetonitrile, dissolve in water and dilute to 100mL, mix well.
5.2.2 80% dichloromethane methanol solution. Take 80mL of dichloromethane, add 20mL of methanol, and mix well.
5.2.3 Mobile phase A. take 100mL of water, add 0.1mL of formic acid, and mix well.
5.2.4 Mobile phase B. Take 100 mL of acetonitrile, add 0.1 mL of formic acid, and mix well.
5.3 Standards
Seduramicin (Semduramicin, molecular formula. C45H75O16, CAS number. 113378-31-7), content ≥94.3%.
5.4 Preparation of standard solution
5.4.1 Standard stock solution. Accurately weigh the reference substance equivalent to 10 mg of seduromycin, dissolve it with acetonitrile and dilute it in a 10 mL volumetric flask,
Prepare seduramycin standard stock solution with a concentration of 1 mg/mL, store it below -18 ℃, and have a validity period of 3 months.
5.4.2 10 μg/mL seduromycin standard working solution. Accurately measure 0.1 mL of the standard stock solution into a 10 mL volumetric flask, add 50% acetonitrile
The aqueous solution was diluted to the mark, and prepared into 10 μg/mL seduromycin standard working solution. Stored at 2°C~8°C, the validity period was 1 month.
5.4.3 1 μg/mL seduamycin standard working solution. accurately measure 1.0 mL of 10 μg/mL seduamycin standard working solution in a volume of 10 mL
Dilute to the mark with 50% acetonitrile aqueous solution to prepare 1 μg/mL seduromycin standard working solution. Store at 2°C~8°C, valid for 1
month.
5.5 Materials
5.5.1 Solid phase extraction column. graphitized carbon black amino solid phase extraction column. 500mg/6mL.
5.5.2 Membrane. organic phase, 0.22 μm.
6 Instruments and equipment
6.1 Ultra-high performance liquid chromatography-tandem mass spectrometer. with electrospray ionization source.
6.2 Analytical balance. Sensitivity 0.01g and 0.00001g.
6.3 High speed centrifuge.
6.4 Vortex mixer.
6.5 Horizontal oscillator.
6.6 Homogenizer.
6.7 Solid phase extraction device.
6.8 Nitrogen blowing instrument.
7 Preparation and storage of samples
7.1 Sample preparation
Take an appropriate amount of fresh or thawed blank or test tissue, mince it, and homogenize it.
a) Take the homogenized test sample as the test sample;
b) Take the homogenized blank sample as the blank sample;
c) Take the homogenized blank sample, add the standard working solution of appropriate concentration, and add the sample as a blank.
7.2 Sample storage
Store below -20°C.
8 Measurement steps
8.1 Extraction
Take 2 g of the sample (accurate to ±0.05 g), add 12 mL of acetonitrile to a 50 mL centrifuge tube, vortex and mix for 1 min, shake for 10 min,
Centrifuge at 5000r/min for 5min (liver at 8000r/min), take the supernatant, add acetonitrile 12mL to repeat the extraction once, combine the two extracts,
spare.
8.2 Purification
The extraction column was activated with 5 mL of dichloromethane and 5 mL of acetonitrile in sequence, and the spare solution was taken and passed through the column at a controlled flow rate of 2 mL/min to 3 mL/min.
Drained for 10 min, eluted with 6 mL of 80% dichloromethane methanol solution, collected the eluate, and dried with nitrogen in a water bath at 40°C. Dissolved with 50% acetonitrile in water
The solution was dissolved and diluted to 2.0 mL, filtered, and determined by ultra-high performance liquid chromatography-tandem mass spectrometry.
8.3 Preparation of matrix-matched standard curve
Precisely measure 20 μL, 40 μL and 100 μL of 1 μg/mL sedumecin standard working solution, 10 μg/mL sedumecin standard working solution
20 μL, 100 μL and.200 μL were added to 6 parts of the blank sample residues that were treated according to the extraction and purification process, dissolved in 50% acetonitrile aqueous solution and
Diluted to 2mL, prepared at concentrations of 10ng/mL, 20ng/mL, 50ng/mL, 100ng/mL, 500ng/mL and 1000ng/mL
The matrix matching series standard solutions were centrifuged at 10,000 r/min at 4°C for 10 min, and the supernatant was taken, filtered through a filter membrane, and used for ultra-high performance liquid chromatography-tandem
Mass spectrometry. Take the measured characteristic ion chromatogram peak area as the ordinate, and the matrix matching standard solution concentration as the abscissa, draw the matrix matching standard curve
Line. Find the regression equation and correlation coefficient.
8.4 Determination
8.4.1 Chromatographic reference conditions
a) Chromatographic column. C18 chromatographic column (100mm×2.1mm, 1.7μm), or equivalent;
b) Mobile phase. A is 0.1% formic acid solution, B is 0.1% formic acid acetonitrile solution;
c) Gradient elution. the gradient elution program is shown in Table 1;
d) Flow rate. 0.3mL/min;
e) Column temperature. 30°C;
f) Injection volume. 10 μL.
8.4.2 Reference conditions for mass spectrometry
a) Ion source. electrospray ion source;
b) Scanning mode. positive ion scanning;
c) Detection method. multiple reaction monitoring;
d) Ionization voltage. 3.0kV;
e) Source temperature. 100°C;
f) Atomization temperature. 350°C;
g) Cone gas flow rate. 20L/h;
h) Atomized gas flow rate. 600L/h;
i) Refer to Table 2 for the reference values of test drug qualitative ion pair, quantitative ion pair, cone voltage and collision energy.
8.5 Determination method
Take the sample solution and matrix-matched standard solution for single-point or multi-point calibration, and calculate with the external standard method. Matrix-matched standard solution and sample solution
The characteristic ion mass chromatographic peak areas of seduromycin should be within the linear range of instrument detection. The relative ion abundance in the sample solution and the basic
Compared with the relative ion abundance in the mass-matched standard solution, it meets the requirements of Table 3.The characteristic ion mass chromatogram of the standard solution is shown in Appendix A.
8.6 Blank test
Take the blank sample, except that no drug is added, the same steps are used for parallel operation.
9 Calculation and presentation of results
The residual amount of seduramycin in the sample was calculated according to the formula (1).
10 Detection method sensitivity, accuracy and precision
10.1 Sensitivity
The detection limit of this method was 3 μg/kg, and the limit of quantification was 10 μg/kg.
10.2 Accuracy
The recovery rate of this method was 70%-120% at the spiked concentration level of 10 μg/kg-400 μg/kg.
10.3 Precision
In this method, the relative standard deviation within the batch was ≤20%, and the relative standard deviation between batches was ≤20%.
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