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GB/T 44621-2024Inspection of grain and oils - Determination of fatty-acid-bound 3-chloropropane-1,2-diols (MCPDs) and glycidol by GC/MS (English PDF)

粮油检验 GC/MS法测定3-氯丙醇脂肪酸酯和缩水甘油脂肪酸酯

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

September 29, 2024

Implementation date

April 1, 2025

Scope

GB/T 44621-2024 is the English-translated version of 粮油检验 GC/MS法测定3-氯丙醇脂肪酸酯和缩水甘油脂肪酸酯.

GB/T 44621-2024 is the Chinese standard "Inspection of grain and oils - Determination of fatty-acid-bound 3-chloropropane-1,2-diols (MCPDs) and glycidol by GC/MS".

Its scope clause reads: This document describes the method for the determination of 3-chloropropanol fatty acid esters and glycidyl fatty acid esters, including the test principle, reagents and materials, instrumentation, and Instruments and equipment, sample preparation, test procedures, result calculation, precision, etc. This document applies to the determination of 3-chloropropanol fatty acid esters and glycidyl fatty acid esters in solid and liquid oils.

It is used for the determination of 3-chloropropanol fatty acid esters and glycidyl fatty acid esters in oils and fats. Chapters 5, 6 and 7 are applicable to the determination of 3-chloropropanol fatty acid esters and glycidyl fatty acid esters in oils and fats.

Determination of 2-propanol fatty acid esters, 2-chloropropanol fatty acid esters and glycidyl fatty acid esters. Chapter 5 does not apply to milk and milk products and their fats.

Chapter 7 does not apply to milk and dairy products and their fats, infant formula, emulsifiers, free fatty acids and other oil derivatives. The limit of detection (LOD) of this document is 30µg/kg and the limit of quantification (LOQ) is 100µg/kg. Its clauses include terms and definitions.

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Document preview — GB/T 44621-2024

National Standard of the People's Republic of China

ICS: 67.200.10
Classification: X14

Issued by: State Administration for Market Regulation; Standardization Administration of the PRC

Preface
1 Scope
2 Normative references
3 Terms and Definitions
Appendix A (Informative) Comparison table of structure numbers and technical differences and their causes
Appendix B (Informative) Inter-laboratory Comparison Verification Test Results of the Difference Method
Appendix F (Informative) Results of inter-laboratory comparison and validation test of acid transesterification method
Appendix I (Informative) Chromatogram of calibration sample in rapid alkaline transesterification method
References

1 Scope

This document describes the method for the determination of 3-chloropropanol fatty acid esters and glycidyl fatty acid esters, including the test principle, reagents and materials, instrumentation, and

Instruments and equipment, sample preparation, test procedures, result calculation, precision, etc.

This document applies to the determination of 3-chloropropanol fatty acid esters and glycidyl fatty acid esters in solid and liquid oils.

Determination of 2-propanol fatty acid esters, 2-chloropropanol fatty acid esters and glycidyl fatty acid esters. Chapter 5 does not apply to milk and milk products and their fats.

Chapter 7 does not apply to milk and dairy products and their fats, infant formula, emulsifiers, free fatty acids and other oil derivatives.

The limit of detection (LOD) of this document is 30µg/kg and the limit of quantification (LOQ) is 100µg/kg.

2 Normative references

The contents of the following documents constitute 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 6682-2008, ISO 3696.1987, MOD)1)

1) ISO 3696.1987 has been superseded by ISO 3696.2021.

GB/T 15687 Preparation of animal and vegetable fats and oils samples (GB/T 15687-2008, ISO 661.2003, IDT)

3 Terms and definitions

There are no terms or definitions that require definition in this document.

4 Rapid alkaline transesterification for determination of 3-MCPD and differential determination of glycidol (referred to as differential method)

4.1 Principle

This method consists of two experimental parts. After base-catalyzed ester cleavage, 3-chloropropanol fatty acid ester and glycidol fatty acid ester are respectively

In test (A), an acidic aqueous solution of sodium chloride was added to convert glycidol into 3-chloropropanol.

In the test (B), an acidic aqueous solution of sodium bromide was added to convert glycidol into 3-bromopropanol; after derivatization with phenylboronic acid, a gas chromatography-mass spectrometry (GC-MS) was performed.

Spectral analysis, internal standard method for quantification; Test (A) 3-chloropropanol content is used to express the content of 3-chloropropanol fatty acid esters and glycidyl fatty acid esters in the sample

The content of 3-chloropropanol fatty acid ester in the sample is expressed as 3-chloropropanol; the content of glycidyl fatty acid ester in the sample is expressed as the sum of the two

The content of glycidyl fatty acid ester was calculated from the conversion rate of glycidol to 3-chloropropanol, which was proportional to the difference (AB) of some tests.

4.2 Reagents and materials

Unless otherwise specified, all reagents used are analytically pure reagents; the test water should comply with the requirements of Grade 1 water in GB/T 6682.

4.2.1 Toluene

chromatographic grade.

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 50 pages — is available in the English PDF.

Referenced standards

Normative references

ISO 3696.1987 · ISO 3696.2021 · ISO 661.2003

Similar standards

GB 38031-2025|GB/T44621-2024|GB/T 1.1-2020|GB/T 6682|GB/T 6682-2008|GB/T 15687|GB/T 15687-2008|GB/T 6682.

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