Determination method of 1-deoxynojirimycin content in silkworm powder

Abstract

A determination method of the 1-deoxynojirimycin content in silkworm powder relates to silkworm powder. The method comprises the following steps: weighing two 1-deoxynojirimycin control samples used as control liquid 1 and 2; sucking the control liquid 1 and 2, injecting the samples; weighing silkworm powder to be determined, adding petroleum ether, performing heating reflux and extraction in water bath, filtering, removing the filtrate, volatilizing the petroleum ether to dryness to obtain a product A; adding methanol in A, performing ultrasonic extraction, filtering, concentrating the filtrate, adding in a neutral alumina column, performing elution, collecting the eluted solution, evaporate to dryness, dissolving by methanol and obtaining a constant volume so as to used the solution as a test solution; performing HPLC analysis of the test solution, calculating the 1-deoxynojirimycin content in the silkworm powder to be determined by an external standard two-point method according to a peak area value. The method has the advantages of high precision, good repeatability and stability, qualified sample recovery rate, simplicity and practicality, and the like, can be popularized in general laboratories, and is applicable to the quality control of 1-deoxynojirimycin in silkworm powder products.

Description

technical field [0001] The invention relates to a whole silkworm powder, in particular to a method for determining the content of 1-deoxynojirimycin in whole silkworm powder by reverse-phase high-performance liquid chromatography. Background technique [0002] The 1-deoxynojirimycin in whole silkworm powder is the main active ingredient for lowering blood sugar. 1-Deoxynojirimycin and its derivatives have high-efficiency and extensive pharmacological effects, and have significant therapeutic effects on diabetes and its complications, obesity, and viral infection (HIV). How to effectively detect the quality of 1-deoxynojirimycin products and create a simple, fast and efficient method for detecting the content of 1-deoxynojirimycin has gradually become one of the research hotspots. There are four main methods for determining the content of 1-deoxynojirimycin: [0003] The first is the ion chromatography method. Chen Zhiyi et al. used this method to quantitatively analyze 1-d...

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Problems solved by technology

The results show that the ion chromatography method has the advantages of simple sample processing and easy operation, but the separation effect and reliability are not ideal; the reversed-phase high performance liquid chromatography-fluorescence detection method has the advantages of high sensitivity, accurate and reliable results, etc., but requires Advanced detectors are expensive, and are rarely configured in general laboratories, which are greatly limited in terms of application popularity.

[0005] The third is reversed-phase high-performance liquid chromatography-ultraviolet detection. Although the detectors used in this method are popular in most laboratories, the samples need to be derivatized before the column. The derivatization process is complicated and the conditions are difficult to grasp.

[0006] The fourth is to use an evaporative light scattering detector to measure 1-deoxynojirimycin in silkworms, which is not as sensitive as ultraviolet detectors and fluorescence detectors

[0007] The detection of 1-deoxynojirimycin content in whole silkworm powder by ultraviolet terminal absorption method has not been reported at home and abroad.

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