Technical requirements for the development and calibration of Chinese medicine reference materials (1)

The main technical aspects of the development and calibration of Chinese medicine reference materials include: species identification, candidate raw material preparation technology research, candidate raw material calibration, and value research, etc.

1.

(1) Determination of variety

According to the needs of the formulation or revision of national drug standards, determine the varieties of chemical reference substances

(2) Investigation on the acceptance of drug standards

Use reference retrieval, usage and corresponding chromatographic conditions from the current pharmaceutical standards ( "Chinese Pharmacopoeia" national drug standards or drug registration standards)

The purity analysis and content determination methods used in the calibration method should cover the methods used in the standard as much as possible, and refer to the 2015 edition of the "Chinese Pharmacopoeia" Four General Principles and the "Chinese Drug Inspection Standard Practice".

(3) Requirements for candidate raw materials for chemical reference substances of traditional Chinese medicine

For the raw materials provided for the first time, the raw material supplier shall provide detailed structure research data, purity research data and stability influencing factors research data

1.

2.

3.

4.

(4) Calibration content and method

1.

2.

3.

4.

(1) Thin-layer chromatography (TLC): The thin-layer plate, developing agent, spot size, detection methods and test conditions should be investigated, and analytical methods with large capacity, good resolution and sensitive detection should be selected

(2) High performance liquid chromatography (HPLC): The chromatographic conditions (including chromatographic column, mobile phase, injection volume, flow rate, column temperature, etc.

(3) Gas Chromatography (GC): The chromatographic conditions (including chromatographic column, inlet temperature, column temperature, carrier gas flow rate, detection method, detection temperature, etc.
) should be investigated, and the chromatographic conditions with good resolution should be selected.
The peak area is compared to determine the purity
.

(5) The fixed value of Chinese medicine chemical reference substance

The fixed value of the chemical reference substance of traditional Chinese medicine mainly adopts the mass balance method, that is, the total content of the main component, moisture, organic solvent, inorganic impurity, and organic impurity content of a chemical reference substance should be 100.
0%, and the fixed value formula is: content (%) =(100.
0-moisture-organic solvent-inorganic impurities)×chromatographic purity×100%
.
In order to ensure the accuracy of the measurement value, other methods in the "external standard method, volumetric analysis method, differential scanning calorimetry, etc.
" are also used to assist and prove the measurement value of the mass balance method, and extensive collaborative calibration work should be carried out
.

1.
The chemical reference substance for identification is only a chemical reference substance for identification or system suitability test, and does not involve the use of value
.
This type of reference substance does not give a definite value .

2.
The chemical reference substance for content determination shall be given a quantitative value in accordance with the mass balance method, and the use method of the variety shall be determined through experiments according to the characteristics of the variety
.
It is mainly divided into three categories: do not need to be dried before use, use after drying under specified temperature conditions, and self-test moisture before use
.

Related Links: General Overview of Drug Reference Materials (2)