GB/T 32951-2016Determination of oxytetracyline, tetracyline, chlortetracycline and doxycycline content for organic fertilizers—HPLC method (English PDF)
有机肥料中土霉素、四环素、金霉素与强力霉素的含量测定 高效液相色谱法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
August 29, 2016
Implementation date
March 1, 2017
Scope
GB/T 32951-2016 is the English-translated version of 有机肥料中土霉素、四环素、金霉素与强力霉素的含量测定 高效液相色谱法.
GB/T 32951-2016 fixes a high performance liquid chromatography method for determining the content of oxytetracycline, tetracycline, chlortetracycline and doxycycline in organic fertilizers.
Clause 1 says it applies to the determination of those four substances in organic fertilizers and in organic-inorganic compound fertilizers, and it states expressly that it does not apply to their determination in soybean cake fertilizer.
The same clause gives the detection limits of the method as 0.75 mg/kg for oxytetracycline, 0.75 mg/kg for tetracycline and 1.0 mg/kg for chlortetracycline, and a fourth limit of 0.75 mg/kg whose analyte name the draft garbles.
A warning at the head of the text notes that applying the standard may involve hazardous materials, operations and equipment, that it does not address every related question, and that the user is responsible for establishing safety and protective measures and for deciding which regulations apply.
The page shows no contents list; in the body, clause 2 cites GB/T 6379.1, GB/T 6379.2 and GB/T 6682, clause 3 sets out the principle, in which the four compounds are extracted with an extractant of Na2EDTA and methanol, whose third component the draft garbles, cleaned up on a solid phase extraction column and then injected and determined by high performance liquid chromatography with a UV detector, quantified against external standards, and clause 4 lists the reagents and materials, requiring analytical grade reagents and water of the first grade specified in GB/T 6682 and naming chromatography-pure methanol and acetonitrile, disodium hydrogen phosphate, citric acid, disodium EDTA and hydrated oxalic acid, together with a 0.4 mol/L disodium hydrogen phosphate solution and a 0.2 mol/L citric acid solution and the weighings used to prepare them.
The draft breaks off inside that reagent list, so the sampling, instrument and measurement clauses are not displayed.
The standard was proposed by the China Petroleum and Chemical Industry Association and is held by the National Technical Committee on Standardization of Fertilizers and Soil Conditioners (SAC/TC105), and it was drafted by the Shanghai Chemical Industry Research Institute, the industrial products and raw materials testing technology centre of the Shanghai Entry-Exit Inspection and Quarantine Bureau, the Taizhou City product quality supervision and inspection institute and Shanghai Jiaotong University.
It carries ICS 65.080 and Chinese classification G20, and it was issued on 29 August 2016 and has applied since 1 March 2017.
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Document preview — GB/T 32951-2016
National Standard of the People's Republic of China
- ICS
- 65.080
- Classification
- G 20
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Foreword
- 1 Scope
- 2 Normative reference documents
- 3 Principle
- 4 Reagents and materials
Foreword
This standard is drafted in accordance with the rules given in GB/T 1.1-2009.
1 Scope
This standard specifies the high performance liquid chromatography (HPLC) method for the determination of oxytetracycline, tetracycline, chlortetracycline and doxycycline in organic fertilizers.
This standard is applicable to the determination of oxytetracycline, tetracycline, chlortetracycline and doxycycline in organic fertilizers and organic-inorganic compound fertilizers.
This standard does not apply to the determination of oxytetracycline, tetracycline, chlortetracycline and doxycycline in soybean cake fertilizer.
The detection limits of this method are. oxytetracycline 0.75mg/kg, tetracycline 0.75mg/kg, chlortetracycline 1.0mg/kg, strong mold The amount of 0.75mg/kg.
2 Normative reference documents
The following documents are indispensable for the application of this document. For dated references, only the dated edition applies to this document. For undated references, the latest edition (including all modifications) applies to this document.
GB/T 6379.1 Accuracy of measurement methods and results (accuracy and precision) - Part 1: General and definitions
GB/T 6379.2 Accuracy of measurement methods and results (accuracy and precision) - Part 2: Determination of standard measurement methods The basic method of sex and reproducibility
GB/T 6682 Analytical laboratory water specifications and test methods
3 Principle
The oxytetracycline, tetracycline, chlortetracycline and doxycycline were extracted by Na2EDTA-Mclvaine-methanol extract, and the solid phase extraction column Purification treatment after injection, high performance liquid chromatography UV detector determination, external standard quantitative.
4 Reagents and materials
Unless otherwise stated, all reagents are of analytical grade and water is a primary water specified in GB/T 6682.
4.1 Methanol. pure chromatography.
4.2 Acetonitrile. pure chromatography.
4.3 disodium hydrogen phosphate (Na2HPO4 . 12H2O).
4.4 Citric acid (C6H8O7 . H2O).
4.5 disodium EDTA (Na2EDTA . 2H2O).
4.6 Hydrated oxalic acid (C2H2O4 . 2H2O).
4.7 disodium hydrogen phosphate solution. 0.4mol/L. Weigh 143.26g disodium hydrogen phosphate, dissolved in water, volume to 1000mL.
4.8 citric acid solution. 0.2mol/L. Weigh 42.03g citric acid, dissolved in water, set to 1000mL.
......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.
Referenced standards
Normative references
- GB/T 6379.1Accuracy (trueness and precision) of measurement methods and results -- Part 1: General principles and definitions
- GB/T 6379.2Accuracy (trueness and precision) of measurement methods and results - Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method
- GB/T 6682Water for analytical laboratory use - Specification and test methods
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Related Standards
GB/T 6379.1-2004 — Accuracy (trueness and precision) of measurement methods and results -- Part 1: General principles and definitions
GB/T 6379.2-2004 — Measurement methods and results -- Accuracy (trueness and precision) -- Part 2: Determine the standard methods of measurement repeatability and reproducibility of the basic method
GB/T 6379.2-2026 — Accuracy (trueness and precision) of measurement methods and results - Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method
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