Volatile component measuring method for Tibetan medicine heracleum millefolium diels

Abstract

The invention provides a volatile component measuring method for Tibetan medicine heracleum millefolium diels. The method adopts headspace, gaseous phase, and mass spectrum to analyze the volatile components of the powder samples for heracleum millefolium diels root, stem, leaf and flower. The method includes: 1) sample crushing; 2) headspace sample introducing, solvent-free balancing, headspace air quantitative sampling and sample introducing; 3) GC-MS system separate measuring to obtain GC-MS data and 4) processing and analyzing according to GC-MS data, after retrieval by NIST11.L mass spectrum data system, ascertaining the volatile components. The method has the effects of medicinal material crushing, simple to operate, solvent free headspace condition. The method avoids distorting the measuring information caused by different solubility of volatile components. Quick headspace sample introduction and high degree of automation enhances the efficiency and accuracy of quantitative analyses. The result is reliable, and is combined with the spectrum library to retrieve; the method quickly ascertains volatile components. Ascertaining the volatile components in heracleum millefolium diels has significances for studying the material basis of medicinal efficacy, for quality control, for exploiting modern Tibet medicine.

Description

technical field

[0001] The invention belongs to the detection technology of medicinal materials, and in particular relates to a method for measuring the volatile components of the Tibetan medicinal material Rhododendron chinensis by combined headspace-gas phase-mass spectrometry (HS-GC-MS). Background technique

[0002] Heracleum millefolium Diels is a genus of Umbelliferae (Umbelliferae), also known as Tibetan Angelica and Qianye Duhuo. It is produced in my country's Tibet, Qinghai, Gansu, Sichuan, and Yunnan, and belongs to high-altitude medicinal materials. Lianye Duhuo inherits the characteristics of Tibetan medicine with fast effect, strong medicinal power, pure, natural, and non-polluting. It is used as medicine with dried whole herbs.

[0003] There are few research reports on the chemical constituents of the Tibetan medicinal herb C. At present, only Rao Gaoxiong et al. reported (Rao Gaoxiong, Pu Fading, Sun Handong. The chemical composition and taxonomic significan...

Examples

Embodiment 1

[0037] The method for the determination of volatile components in the root of the Tibetan medicinal material Lola lobata comprises the following steps:

[0038] 1) Sample pulverization: take the root of the lobster leaf and pulverize it into medicinal material powder (through a 200-mesh sieve);

[0039] 2) Headspace sampling: Weigh 0.2000 g of the above medicinal material powder, put it directly into a 20 ml headspace bottle and seal it in a sample tray. The heating temperature of the sample vial is 100 °C, and the equilibration time is 40 min; 1 mL of the gas in the headspace of the vial is injected into the GC-MS system, the temperature of the quantitative loop is 120 °C, and the temperature of the transfer line is 140 °C;

[0040] 3) Separation and detection by GC-MS system: separation by gas chromatography and detection by mass spectrometry.

[0041] Among them, gas chromatography conditions: HP-5 capillary column elastic chromatography column (0.25μm×250μm×30m); carrier ...

Embodiment 2

[0046] The determination method of the volatile components in the stems of the Tibetan medicinal herb L. chinensis comprises the following steps:

[0047] 1) Sample pulverization: take the stem of the lobed leaf and pulverize it into medicinal material powder (through a 300-mesh sieve);

[0048]2) Headspace sampling: Weigh 0.2500 g of the above medicinal material powder, put it directly into a 20 ml headspace bottle and seal it in a sample tray. The heating temperature of the sample bottle is 60°C, and the equilibration time is 120min; 1mL of the gas in the headspace of the sample bottle is injected into the GC-MS system, the temperature of the quantitative loop is 80°C, and the temperature of the transfer line is 100°C;

[0049] 3) Separation and detection by GC-MS system: separation by gas chromatography and detection by mass spectrometry.

[0050] Among them, gas chromatography conditions: HP-5 capillary column elastic chromatography column (0.25μm×250μm×30m); carrier gas:...

Embodiment 3

[0054] The method for the determination of volatile components in the leaves of the Tibetan medicinal herb Cracked Leaf, comprises the following steps:

[0055] 1) Sample pulverization: take the leaves of Cracked Leaves and pulverize them into medicinal material powder (pass through a 400-mesh sieve);

[0056] 2) Headspace sampling: Weigh 0.1500 g of the above medicinal material powder, put it directly into a 20 ml headspace bottle and seal it in a sample tray. The heating temperature of the sample vial is 200 °C, and the equilibration time is 10 min; 1 mL of the gas in the headspace of the vial is injected into the GC-MS system, the temperature of the quantitative loop is 180 °C, and the temperature of the transfer line is 180 °C;

[0057] 3) Separation and detection by GC-MS system: separation by gas chromatography and detection by mass spectrometry.

[0058] Among them, gas chromatography conditions: HP-5 capillary column elastic chromatography column (0.25μm×250μm×30m); c...

technical field

[0001] The invention belongs to the detection technology of medicinal materials, and in particular relates to a method for measuring the volatile components of the Tibetan medicinal material Rhododendron chinensis by combined headspace-gas phase-mass spectrometry (HS-GC-MS). Background technique

[0002] Heracleum millefolium Diels is a genus of Umbelliferae (Umbelliferae), also known as Tibetan Angelica and Qianye Duhuo. It is produced in my country's Tibet, Qinghai, Gansu, Sichuan, and Yunnan, and belongs to high-altitude medicinal materials. Lianye Duhuo inherits the characteristics of Tibetan medicine with fast effect, strong medicinal power, pure, natural, and non-polluting. It is used as medicine with dried whole herbs.

[0003] There are few research reports on the chemical constituents of the Tibetan medicinal herb C. At present, only Rao Gaoxiong et al. reported (Rao Gaoxiong, Pu Fading, Sun Handong. The chemical composition and taxonomic significan...

Examples

Embodiment 1

[0037] The method for the determination of volatile components in the root of the Tibetan medicinal material Lola lobata comprises the following steps:

[0038] 1) Sample pulverization: take the root of the lobster leaf and pulverize it into medicinal material powder (through a 200-mesh sieve);

[0039] 2) Headspace sampling: Weigh 0.2000 g of the above medicinal material powder, put it directly into a 20 ml headspace bottle and seal it in a sample tray. The heating temperature of the sample vial is 100 °C, and the equilibration time is 40 min; 1 mL of the gas in the headspace of the vial is injected into the GC-MS system, the temperature of the quantitative loop is 120 °C, and the temperature of the transfer line is 140 °C;

[0040] 3) Separation and detection by GC-MS system: separation by gas chromatography and detection by mass spectrometry.

[0041] Among them, gas chromatography conditions: HP-5 capillary column elastic chromatography column (0.25μm×250μm×30m); carrier ...

Embodiment 2

[0046] The determination method of the volatile components in the stems of the Tibetan medicinal herb L. chinensis comprises the following steps:

[0047] 1) Sample pulverization: take the stem of the lobed leaf and pulverize it into medicinal material powder (through a 300-mesh sieve);

[0048]2) Headspace sampling: Weigh 0.2500 g of the above medicinal material powder, put it directly into a 20 ml headspace bottle and seal it in a sample tray. The heating temperature of the sample bottle is 60°C, and the equilibration time is 120min; 1mL of the gas in the headspace of the sample bottle is injected into the GC-MS system, the temperature of the quantitative loop is 80°C, and the temperature of the transfer line is 100°C;

[0049] 3) Separation and detection by GC-MS system: separation by gas chromatography and detection by mass spectrometry.

[0050] Among them, gas chromatography conditions: HP-5 capillary column elastic chromatography column (0.25μm×250μm×30m); carrier gas:...

Embodiment 3

[0054] The method for the determination of volatile components in the leaves of the Tibetan medicinal herb Cracked Leaf, comprises the following steps:

[0055] 1) Sample pulverization: take the leaves of Cracked Leaves and pulverize them into medicinal material powder (pass through a 400-mesh sieve);

[0056] 2) Headspace sampling: Weigh 0.1500 g of the above medicinal material powder, put it directly into a 20 ml headspace bottle and seal it in a sample tray. The heating temperature of the sample vial is 200 °C, and the equilibration time is 10 min; 1 mL of the gas in the headspace of the vial is injected into the GC-MS system, the temperature of the quantitative loop is 180 °C, and the temperature of the transfer line is 180 °C;

[0057] 3) Separation and detection by GC-MS system: separation by gas chromatography and detection by mass spectrometry.

[0058] Among them, gas chromatography conditions: HP-5 capillary column elastic chromatography column (0.25μm×250μm×30m); c...

Images