GB/T 19427-2022Determination of 12 phenolic compounds in propolis— HPLC-MS/MS method and HPLC method (English PDF)

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 of Standardization Documents" drafted.

This document replaces GB/T 19427-2003 "Rutin, myricetin, quercetin, camphenyl alcohol, apigenin, pinesin, caustic factor, gaoliang in propolis" Determination method of gingerin content liquid chromatography-tandem mass spectrometry detection method and liquid chromatography-ultraviolet detection method", in accordance with GB/T 19427-2003 In addition to structural adjustments and editorial modifications, the main technical changes are as follows.

a) Added the detection items of caffeic acid, p-coumaric acid, ferulic acid, gracilisin 3-acetate, chlorogenic acid, and atipirin C (see Section 1 Chapter, 5.11, 7.2);

b) Deleted the detection items of rutin and myricetone (see Chapter 1, 4.4, 4.5, 4.6, 6.2 of the.2003 edition);

c) Changed the extraction conditions of propolis samples (see 7.1, 6.1 of the.2003 edition).

1 Scope

This document describes the caffeic acid, p-coumaric acid, ferulic acid, quercetin, camphenyl alcohol, apigenin, pinesin, caine, galangin, Liquid chromatography-tandem mass spectrometry and liquid chromatography for the content determination of brevin 3-acetate, chlorogenic acid, and atipirin C.

This document applies to caffeic acid, p-coumaric acid, ferulic acid, quercetin, camphenyl alcohol, apigenin, pinesin, caine, galangin, Determination of the content of raffinin 3-acetate, chlorogenic acid, and atipirin C.

2 Normative references

The contents of the following documents constitute essential provisions of this document through normative references in the text. Among them, dated citations documents, only the version corresponding to that date applies to this document; for undated references, the latest edition (including all amendments) applies to this document.

GB/T 6682 Analysis Laboratory Water Specifications and Test Methods

3 Terms and Definitions

There are no terms and definitions that need to be defined in this document.

4 Principles

Propolis sample is extracted with 85% ethanol aqueous solution, after ultrasonication, centrifugation, filtration and constant volume, it is determined by liquid chromatography-tandem mass spectrometer or equipped with violet It was determined by liquid chromatograph with external detector and quantified by external standard method.

5 Reagents and Materials

Unless otherwise stated, the reagents used are of analytical grade, and the water is the first grade water specified in GB/T 6682.

5.1 Ethanol. absolute ethanol.

5.2 Methanol. chromatographically pure.

5.3 Formic acid. chromatographically pure.

5.4 Acetic acid. chromatographically pure.

5.5 Aqueous ethanol solution (85 15). accurately pipette 85mL of ethanol (5.1) into a 100mL volumetric flask, and dilute to volume with water.

5.6 Methanol aqueous solution (80 20). accurately pipette 80 mL of methanol (5.2) into a 100 mL volumetric flask, and dilute to volume with water.

5.7 Methanol-0.1% formic acid aqueous solution (50 50). accurately pipette 50 mL methanol (5.2) and 0.1 mL formic acid (5.3) to a volume of 100 mL. In a measuring bottle, make up to volume with water.

5.8 0.1% formic acid aqueous solution. accurately pipette 1.0 mL of formic acid (5.3) into a 1000 mL volumetric flask, and dilute to volume with water.

5.9 0.1% formic acid-methanol solution. accurately pipette 1.0 mL of formic acid (5.3) into a 1000 mL volumetric flask, and dilute to volume with methanol (5.2).

5.10 1.0% acetic acid aqueous solution. accurately pipette 10 mL of acetic acid (5.4) into a 1000 mL volumetric flask, and dilute to volume with water.