CN102139045A - Quality control method for Xiebai syrup - Google Patents

Abstract

The invention relates to a quality control method for Xiebai syrup, which comprises the step of distinguishing the component of menthol crystal through thin-layer chromatography, and specifically comprises the following steps of: (1) preparing a test solution; (2) preparing a reference solution; and (3) regulating thin-layer chromatographic conditions and acquiring results. In the invention, the quality standard of the Xiebai syrup is improved and perfected, a thin-layer distinguishing method of the menthol crystal is increased, and other components are subjected to detection tests; and based on the revised quality standard, the quality control of medicines is improved, therefore the qualitative and quantitative detection of the medicines is more accurate, and the quality is easier to control.

Description

The syrupy method of quality control of purging pathogenic fire of the lung

Technical field

The invention belongs to technical field of Chinese medicines, relate to the detection method of Chinese medicine, the syrupy method of quality control of especially a kind of purging pathogenic fire of the lung.

Background technology

Syrupy main component of purging pathogenic fire of the lung and content are as follows:

[prescription] Gypsum Fibrosum 15g Cortex Mori 10g Semen Trichosanthis 10g

Semen Lepidii (Semen Descurainiae) 5g Herba Ephedrae 10g Radix Glycyrrhizae 10g

Radix Peucedani 15g Radix Asteris 15g Flos Farfarae 10g

Bulbus Fritillariae Cirrhosae 10g Semen Armeniacae Amarum 15g Folium perillae acutae oil 0.048ml

Mentholum 0.05g

Preparation method is: above 13 flavors, it is standby that Semen Armeniacae Amarum extracts aqua armeniacae: Gypsum Fibrosum, Radix Peucedani, Radix Asteris, Flos Farfarae, Cortex Mori, Semen Trichosanthis, Semen Lepidii (Semen Descurainiae), Herba Ephedrae, Radix Glycyrrhizae, Bulbus Fritillariae Cirrhosae decoct with water twice, 2 hours for the first time, collect distillate 120ml simultaneously, 1 hour for the second time, collecting decoction is concentrated in right amount, use ethanol precipitation, leave standstill, filter, reclaim ethanol, be concentrated into an amount of.With distillate, concentrated solution mixing, leave standstill, filter, add with the Folium perillae acutae oil of an amount of dissolve with ethanol and Mentholum alcoholic solution and aqua armeniacae, simple syrup, mixing, the adjustment capacity is measured relative density 1.15～1.20 (25 ℃), makes 1000ml, fill, that is, and every bottled 10ml.

Function with cure mainly: lung qi dispersing is analgesic, and preventing phlegm from forming and stopping coughing is used for the cough due to common cold, the abundant expectoration fullness in the chest, thirsty dry tongue, it is obstructed to have a stuffy nose.

Summary of the invention

The objective of the invention is to overcome the deficiencies in the prior art part, a kind of syrupy method of quality control of purging pathogenic fire of the lung that can the qualitative detection ingredient is provided, this method has that detection means is simple, testing result characteristic of accurate more.

The objective of the invention is to be achieved through the following technical solutions:

The syrupy method of quality control of a kind of purging pathogenic fire of the lung, the step of its method is: thin layer chromatography differentiates that the step of Mentholum composition is:

1. the preparation of need testing solution: get purging pathogenic fire of the lung syrup sample, add chloroform extraction three times, each 20ml merges the chloroform layer, and 40 ℃ volatilize to about 0.5ml, as need testing solution;

2. the preparation of reference substance solution: get the Mentholum reference substance, add ethanol and make the solution that every 1ml contains the 2mg Mentholum, in contrast product solution;

3. thin layer chromatography condition and result: draw above-mentioned need testing solution 8-10 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with petroleum ether: ethyl acetate=5: 1 is developing solvent, launches, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing at 105 ℃, inspect in the test sample chromatograph with the corresponding position of reference substance chromatograph on whether show the speckle of same color, determine whether contain the Mentholum composition in the test sample.

Advantage of the present invention and good effect are:

The present invention has carried out raising, perfect to purging pathogenic fire of the lung syrup quality standard, increased the thin layer discrimination method of Mentholum, and to other compositions test experience in addition, owing to detect the restriction of effect, do not include this method of quality control in, revised quality standard has improved the quality control of medicine, make the qualitative and detection by quantitative of medicine more accurate, quality is more prone to control.

Description of drawings

The chromatogram that Fig. 1 differentiates for Mentholum thin layer chromatography of the present invention, be followed successively by from left to right: 1, Mentholum reference substance, 2, purging pathogenic fire of the lung syrup sample (lot number: 0712199), 3, purging pathogenic fire of the lung syrup sample (lot number: 0712200), 4, purging pathogenic fire of the lung syrup sample (lot number: 0712201), 5, Mentholum negative control, 6, the Mentholum reference substance.

The specific embodiment

Below in conjunction with embodiment, the present invention is further described, and following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.

The syrupy method of quality control of a kind of purging pathogenic fire of the lung, the step of its method is:

(1) thin layer chromatography of Mentholum is differentiated

1. the preparation of need testing solution: get purging pathogenic fire of the lung syrup sample 20ml, add chloroform extraction three times, each 20ml merges the chloroform layer, and 40 ℃ volatilize to about 0.5ml, as need testing solution;

2. the preparation of reference substance solution: get the Mentholum reference substance, add ethanol and make the solution that every 1ml contains the 2mg Mentholum, in contrast product solution;

3. the preparation of negative sample solution: by the prescription proportioning, get other flavor medical materials of removing Mentholum, make sample, make negative sample solution by above-mentioned need testing solution preparation method again by the technology under the method for making item;

4. thin layer chromatography condition and result: according to thin layer chromatography (2005 editions appendix VIB of Chinese Pharmacopoeia) test, draw above-mentioned need testing solution 8 ~ 10 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, so that petroleum ether (60 ℃ ~ 90 ℃)-ethyl acetate (5: 1) is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing at 105 ℃, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color, see Fig. 1.

In experimentation, the applicant has also done following identification experiment, but because identification result is undesirable, so do not include quality standard in, comprising: the thin layer chromatography of Radix Asteris is differentiated, the thin layer chromatography of Cortex Mori is differentiated, the thin layer chromatography of Bulbus Fritillariae Cirrhosae is differentiated, the thin layer chromatography of Folium perillae acutae oil is differentiated, the ephedrine hydrochloride assay.

Claims (1)

1. syrupy method of quality control of purging pathogenic fire of the lung, it is characterized in that: the step of its method is: thin layer chromatography differentiates that the step of Mentholum composition is:

1. the preparation of need testing solution: get purging pathogenic fire of the lung syrup sample, add chloroform extraction three times, each 20ml merges the chloroform layer, and 40 ℃ volatilize to 0.5ml, as need testing solution;

2. the preparation of reference substance solution: get the Mentholum reference substance, add ethanol and make the solution that every 1ml contains the 2mg Mentholum, in contrast product solution;

3. thin layer chromatography condition and result: draw above-mentioned need testing solution 8-10 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with petroleum ether: ethyl acetate=5: 1 is developing solvent, launches, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing at 105 ℃, inspect in the test sample chromatograph with the corresponding position of reference substance chromatograph on whether show the speckle of same color, determine whether contain the Mentholum composition in the test sample.

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