Method for Determination of Index Components in Sishen Pills by Flash Gas Chromatography

A technology of gas chromatograph and Sishen Pills, which is applied in the field of determination of index components in Sishen Pills by flash gas chromatography, can solve the problems of cumbersome extraction process and increased detection workload, and achieve simplified experimental steps and quality evaluation Far-reaching, time-saving effects

Active Publication Date: 2019-11-29
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Existing literature is to the detection method of psoralen and isopsoralen in psoralen and schisandrol A in schisandra chinensis, commonly used methods have thin-layer chromatography, liquid chromatography, gas chromatography etc. The dehydrodiisoeugenol and evodiamine and evodiamine in Evodia rutaecarpa adopt thin-layer chromatography and liquid chromatography; however, cumbersome pretreatment methods such as supercritical extraction and ultrasonic extraction are required
The determination of these substances in Sishen Pill samples is usually performed by liquid chromatography. In addition to the tedious extraction process, the detection of different substances requires different detection wavelengths, which further increases the detection workload.

Method used

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  • Method for Determination of Index Components in Sishen Pills by Flash Gas Chromatography
  • Method for Determination of Index Components in Sishen Pills by Flash Gas Chromatography
  • Method for Determination of Index Components in Sishen Pills by Flash Gas Chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: Qualitative analysis of psoralen, isopsoralen, dehydrodiisoeugenol, schisandrol A, evodiamine and evodiamine in Sishen Pill samples

[0029] (1) Instruments and reagents

[0030] American ThermoFinnigan Trace DSQ gas chromatography / mass spectrometer (GC-MS); American ThermoFinniganTrace GC Ultra gas chromatograph with hydrogen flame detector (FID); Japanese Frontier PY-3030D double-click vertical micro-furnace cracker.

[0031] Purchase local samples of Sishen Pills from various pharmacies, pass through a 120-mesh sieve after grinding, and dry at 60°C to constant weight for later use.

[0032] (2) Experimental method

[0033] Accurately weigh 0.5 mg of Sishen Pill sample (Sishen Pill 1) powder, put it into a sample cup, fix it on the injection rod, and put it into the cracker installed above the GC inlet. At this time, the sample is at room temperature. After the temperature of the cracker reaches the appropriate temperature, press the sample injection butt...

Embodiment 2

[0041] Embodiment 2: the investigation of reproducibility

[0042] American Thermo Trace GC ultra gas chromatograph (TRB-5 metal capillary column, 30m × 0.25mmi.d. × 0.25μm, film thickness 5% methyl polysiloxane, the United States), Japan Frontier PY-3030D double-click vertical type Micro Furnace Cracker.

[0043] Gas phase conditions: heating program: initial temperature 50°C, rise to 200°C at a rate of 10°C / min, then rise to 300°C at a rate of 5°C / min, and keep for 10 minutes; the temperature of the injection port is 300°C, and the temperature of the detector is 300°C ℃, split ratio 30:1; carrier gas nitrogen or helium, flow rate 1.0mL / min.

[0044] Cracker conditions: cracking furnace temperature: 300°C; interface temperature between cracker and gas chromatograph: 300°C.

[0045] Accurately weigh 3 parts of 0.5 mg of the same Sishen Pill 1 sample as in Example 1 and put it into a sample cup, fix it on the injection rod, and put it into the cracker installed above the GC i...

Embodiment 3

[0047] Example 3: Development of Flash Gas Chromatography Methodology for 6 Index Substances in Sishen Pills

[0048] The gas chromatograph of ThermoFinnigan Trace in the United States and the Japan Frontier PY-3030D double-click vertical micro-furnace cracker.

[0049] The gas phase conditions are: the chromatographic column is a TRB-5 quartz capillary column (30m × 0.25mmi.d. × 0.25μm, film thickness 5% methyl polysiloxane, the United States). Raise to 200°C at a rate of ℃ / min, then rise to 300°C at a rate of 5°C / min, and hold for 10 minutes; the temperature of the injection port is 300°C, the temperature of the detector is 300°C, and the split ratio is 30:1; the carrier gas is nitrogen or Helium, flow rate 1.0mL / min.

[0050] Cracker conditions: cracking furnace temperature: 300°C; interface temperature between cracker and gas chromatograph: 300°C.

[0051] Psoralen, isopsoralen and schisandrol A standard substance are made into 20-10000mg / L dichloromethane solution (mixe...

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Abstract

The invention provides a method for simultaneously determining psoralen, isopsoralen, dehydrodiisoeugenol, schizandrol A, evodiamine and rutaecarpine in a Sishen pill through a flash evaporation-gas chromatography technology. The method comprises the following steps: carrying out flash evaporation-gas chromatography detection on a Sishen pill sample to obtain a qualitative analysis result, carrying out an external standard technology to establish a standard working curve, and acquiring quantitative analysis results of the index components in the Sishen pill sample. The method adopting the flash evaporation-gas chromatography to realize the direct introduction of a solid sample without a complex extraction process or a solvent, so the method is simple to operate, and is environmentally-friendly; and the method adopting the flash evaporation-gas chromatography to quantitatively detect the index components in the Sishen pill can effectively save the experiment time and simplify experiment steps, so the above quality evaluation method has the characteristics of simplicity, environmental friendliness and high efficiency, and is of very far-reaching significance to evaluate the quality of the Sishen pill.

Description

[0001] (1) Technical field [0002] The invention relates to a method for determining index components in Sishen Pills by flash gas chromatography, in particular to a method for simultaneously determining psoralen, isopsoralen, and dehydrodiphenhydramine in Sishen Pills by flash gas chromatography. Methods of isoeugenol, schisandrin A, evodiamine and evodiamine. [0003] (2) Background technology [0004] Sishen Pill is the name of a Chinese patent medicine. It is an astringent agent. It has the effects of warming the kidney and dispelling cold, astringent intestines and relieving diarrhea. It is used for diarrhea caused by deficiency of kidney yang. Insufficient appetite, prolonged diarrhea, yellow complexion and cold limbs. Sishen Pill is made from nutmeg, psoralen, schisandra, evodia and jujube, raw gum. Warming the spleen and stomach, astringent intestines and antidiarrheal are all ministerial medicines; Schisandra astringent and astringent are adjuvant drugs; [0005] "...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/12G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/12G01N30/72G01N30/8631G01N2030/126
Inventor 王丽丽黄翌磊黄忠平刘会君
Owner ZHEJIANG UNIV OF TECH
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