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Determination of oxytetracycline in feeds
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Determination of oxytetracycline in feeds -- High performance liquid chromatography
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Basic data
| Standard ID | GB/T 22259-2025 (GB/T22259-2025) |
| Description (Translated English) | Determination of oxytetracycline in feeds |
| Sector / Industry | National Standard (Recommended) |
| Classification of Chinese Standard | B46 |
| Classification of International Standard | 65.120 |
| Word Count Estimation | 14,119 |
| Date of Issue | 2025-08-01 |
| Date of Implementation | 2026-02-01 |
| Older Standard (superseded by this standard) | GB/T 22259-2008 |
| Issuing agency(ies) | State Administration for Market Regulation, Standardization Administration of China |
GB/T 22259-2025: Determination of oxytetracycline in feeds
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT22259-2025
ICS 65.120
CCSB46
National Standard of the People's Republic of China
Replaces GB/T 22259-2008
Determination of oxytetracycline in feed
Released on August 1, 2025
Implementation on February 1, 2026
State Administration for Market Regulation
The National Standardization Administration issued
Preface
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 replaces GB/T 22259-2008 "Determination of oxytetracycline in feed - High performance liquid chromatography method" and is incompatible with GB/T 22259-2008.
In addition to structural adjustments and editorial changes, the main technical changes are as follows.
a) The scope of application, detection limit and quantification limit have been changed (see Chapter 1, Chapter 1 of the.2008 edition);
b) Liquid chromatography-tandem mass spectrometry has been added (see Chapter 4);
c) The principle has been changed (see 5.1, Chapter 3 of the.2008 edition);
d) The reagents or materials have been changed (see 5.2, Chapter 4 of the.2008 edition);
e) The instrumentation has been changed (see 5.3, Chapter 5 of the.2008 edition);
f) The sample has been changed (see 5.4, Chapter 6 of the.2008 edition);
g) The test steps have been changed (see 5.5, Chapter 7 of the.2008 edition);
h) The test data processing has been changed (see 5.6, Chapter 8 of the.2008 edition).
Please note that some of the contents of this document may involve patents. The issuing organization of this document does not assume the responsibility for identifying patents.
This document is proposed and coordinated by the National Feed Industry Standardization Technical Committee (SAC/TC76).
This document was drafted by. Henan Agricultural, Animal and Aquatic Products Inspection Technology Research Institute and Shaanxi Animal Husbandry Technology Extension Center.
The main drafters of this document are. Wu Ningpeng, Peng Li, Li Hong, Li Huisu, Cui Chao, Hu Yanli, Zhang Zhenyu, Zhang Chongwei, Chao Juanjuan, Meng Lei, and Jia Yuhua.
The previous versions of this document and the documents it replaces are as follows.
---First published in.2008 as GB/T 22259-2008;
---This is the first revision.
Determination of oxytetracycline in feed
1 Scope
This document describes a method for the determination of oxytetracycline in feed by liquid chromatography-tandem mass spectrometry and high performance liquid chromatography.
This document applies to compound feeds, concentrated feeds, concentrate supplements, additive premixes, feed ingredients and mixed feed additives
Determination of oxytetracycline in.
The detection limit of this document liquid chromatography-tandem mass spectrometry is 0.02mg/kg and the quantification limit is 0.05mg/kg; high performance liquid chromatography combined with
The detection limit for feed (except aquatic feed), concentrated feed, concentrate supplement and feed raw materials is 1.0 mg/kg and the quantification limit is 2.0 mg/kg.
The detection limit of aquatic feed is 5.0 mg/kg and the quantification limit is 10.0 mg/kg. The limits of detection of premixed feed and mixed feed additives are 5.0 mg/kg and 10.0 mg/kg respectively.
The detection limit is 2.5 mg/kg and the quantification limit is 5.0 mg/kg.
2 Normative references
The contents of the following documents constitute the essential clauses of this document through normative references in this document.
For referenced documents without a date, only the version corresponding to that date applies to this document; for referenced documents without a date, the latest version (including all amendments) applies to
This document.
GB/T 6682 Specifications and test methods for water used in analytical laboratories
GB/T 20195 Preparation of animal feed samples
3 Terms and Definitions
There are no terms or definitions that require definition in this document.
4 Liquid chromatography-tandem mass spectrometry (LC-MS/MS)
4.1 Principle
Oxytetracycline in the sample was extracted with hydrochloric acid methanol solution or buffer solution, the extraction solution was diluted or purified by HLB solid phase extraction column, and the liquid phase was used to extract the oxytetracycline.
The product was determined by chromatography-tandem mass spectrometry, calibrated by matrix-matched standard curve, and quantified by external standard method.
4.2 Reagents or materials
Unless otherwise specified, only analytical grade reagents were used.
4.2.1 Water. GB/T 6682, Grade 1.
4.2.2 Acetonitrile. chromatographic grade.
4.2.3 Methanol. chromatographic grade.
4.2.4 Formic acid. chromatographically pure.
4.2.5 Hydrochloric acid methanol solution. Pipette 20 mL of hydrochloric acid and dissolve it in 1000 mL of methanol and mix well.
4.2.6 Hydrochloric acid solution (1 mol/L). Pipette 9 mL of hydrochloric acid, dilute to 100 mL with water, and mix thoroughly.
4.2.7 Sodium hydroxide solution (1 mol/L). Weigh 4 g of sodium hydroxide, dissolve it in water and dilute to 100 mL, then mix thoroughly.
4.2.8 Buffer Solution I. Weigh 12.9 g of citric acid monohydrate, 27.6 g of disodium hydrogen phosphate dodecahydrate, and 27.6 g of disodium ethylenediaminetetraacetic acid dihydrate.
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