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A kind of detection method of Tibetan medicine crab shell

A detection method, crab nail technology, applied in the field of medicine, can solve the problems of complex operation, multiple peaks, shoulder peaks, inconvenient use, etc., and achieve the effect of simple operation, high resolution and clear spots

Active Publication Date: 2018-12-25
SHANDONG JINHE DRUG RES DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent medicines containing Crab A are "Qiwei Crab A Pill" and "Cuitang Pill", which are respectively implemented in "Drug Standards" (Tibetan Medicine Volume One, 1995 edition) and "Chinese Pharmacopoeia" (2010 edition one). A has only identification items, and its identification and separation effect is not ideal, which cannot fully reflect the quality of crab A medicinal materials
In recent years, there have been many studies on crab shells. For example, "Tin-layer chromatography research on Tibetan medicine reminder soup pills" uses ethanol extraction and chloroform-methanol (6:4) to expand, but the operation is complicated and the expansion effect is not ideal, and chloroform It is inconvenient to use because it is easy to control drug production; "Study on the HPLC Characteristic Map of Tibetan Medicine Crab A" is eluted with acetonitrile-water gradient, and the concentration of acetonitrile changes from 0-8-10-20-40-60-70 minutes, the percentage of acetonitrile The concentration is changed to 0-0-5-5-12.5-100-100 in turn, and 14 characteristic peaks are used, but the gradient is complex, the separation effect of the chromatogram is not ideal, and there are many joint peaks and shoulder peaks. Satisfactory spectra could not be obtained in the experiment (see attached Figure 8 )

Method used

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  • A kind of detection method of Tibetan medicine crab shell
  • A kind of detection method of Tibetan medicine crab shell
  • A kind of detection method of Tibetan medicine crab shell

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0037] Experimental example 1: TLC identification and detection method experiment

[0038]Take three batches of 20150103, 20150204, and 20150301 crab shell medicinal material powder 1g, add ethanol 10ml, heat and reflux for 30 minutes, filter, and the filtrate is used as the test solution; the same method is used to prepare the control medicinal material solution. Take 5 μl of each of the above two solutions and put them on the same silica gel GF254 thin-layer plate, and test according to the thin-layer chromatography method, respectively, using the literature method, that is, chloroform-methanol (volume ratio 6:4), chloroform-methanol-water (volume ratio 13:7:2), petroleum ether (60-90°C) - ethyl acetate - acetone - formic acid (volume ratio 15:15:10:1), chloroform - methanol (9:1), iso Propanol-methanol-formic acid (volume ratio 4:1:0.2), isopropanol-methanol-formic acid (volume ratio 6:1:0.2), isopropanol-methanol-formic acid (volume ratio 8:1:0.2) is Developing agent, dev...

experiment example 2

[0044] Experimental example 2: Obtaining experiment of standard feature map

[0045] 1. Experimental instruments and reagents

[0046] Test equipment: high performance liquid chromatography: Agilent 1260

[0047] Electronic balance: Shimadzu AUW﹣220D

[0048] UV spectrophotometer: Shimadzu UV﹣2450

[0049] Reference substance: Shanzhiside methyl ester reference substance (National Institute for Food and Drug Control) batch number: 111873﹣201103

[0050] Test product: Crab A (provided by Jinhe Tibetan Medicine Co., Ltd.) Batch numbers: 20150101, 20150103, 20150204, 20150205, 20150301, 20150302, 20150303, 20150401, 20150402, 20150403.

[0051] 2. Chromatographic conditions and system suitability test: Octadecylsilane bonded silica gel is used as filler; detection wavelength is 245nm; flow rate: 1.0ml / min; analysis time: 60 minutes.

[0052] Preparation of the reference substance solution: take an appropriate amount of the reference substance of shanzhiside methyl ester, add ...

experiment example 3

[0065] Experimental example 3: Methodological investigation experiment of HPLC characteristic map detection method

[0066] 1. Precision test

[0067] Get batch number and be 20150403 batches of crab first samples, one part of need testing solution that obtains by the preparation method of above-mentioned need testing solution, under the above-mentioned chromatographic conditions continuous sample introduction 5 times is measured, and the result shows: the characteristic spectrum detection method provided by the present invention Precision is good. The measurement results are shown in Table 1.

[0068] Table 1 The precision investigation results of the HPLC characteristic chromatograms of crab beetle (relative retention time)

[0069]

[0070] 2. Repeatability test

[0071] Get batch number and be 20150403 batches of crab first samples, six parts of need testing solution obtained by the preparation method of above-mentioned need testing solution, sample introduction meas...

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Abstract

The present invention provides a detection method for a Tibetan medicine phlomis younghusbandii mukerjee. According to the present invention, a certain proportion of isopropyl alcohol-methanol-formic acid is used as a developing solvent, 254 nm ultraviolet visual inspection and / or sulfuric acid ethanol spraying-heating coloring is selected, the spots on the obtained pattern are clear, and the resolution is high; a phosphoric acid aqueous solution with an acetonitrile-volume fraction ratio of 0.05% is used as a mobile phase, the HPLC characteristic spectrum of the phlomis younghusbandii mukerjee is obtained through gradient elution, and 13 characteristic peaks are determined; and the method has characteristics of simple operation and complete detection, and the obtained characteristic peaks have characteristics of good resolution and clear peak shape.

Description

technical field [0001] The invention relates to a detection method of Tibetan medicine crab shell, which belongs to the technical field of medicine. Background technique [0002] Crab shell is a traditional Tibetan medicinal herb. It comes from the dried root of Phlomis younghusbandii Mukerjee, a perennial herb of the genus Phlomis younghus bandii Mukerjee in the family Lamiaceae. It is called "Lu Muer" in Tibetan and has been used for more than a thousand years. Crab armor has the functions of clearing heat and dispelling wind, moistening throat and dispelling cold, promoting muscle growth and suppressing sores, relieving cough and reducing phlegm. [0003] The medicinal material of crab shellfish is recorded in the "Drug Standards" of the first volume of Tibetan medicine promulgated by the Ministry of Health, the standard number: WS3-BC-0124-95, only the traits, no other identification, inspection and content determination items, the quality standard is urgent Need to imp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/90
Inventor 张义智任松鹏孙绪丁赵延霞魏永义
Owner SHANDONG JINHE DRUG RES DEV
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