Thin-layer chromatographic detection method of curcuma zedoary in Fushengkang tablet

A technique of thin-layer chromatography and detection method, which is applied in the field of thin-layer chromatography detection of Fushengkang Tablets, can solve the problems of high filtration difficulty, poor repeatability, easy gelatinization of ether, etc., and achieves reduction of potential harm and color development Accurate results and consistent results

Inactive Publication Date: 2017-11-07
青岛华仁太医药业有限公司
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  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In addition, the standard zedoary thin-layer chromatography identification method uses ether to sonicate samples, and there are several problems: (1) ether is easy to gelatinize in glassware, making filtration difficult; (2) the filtrate after ultrasonic extraction needs to be volatilized to remove ether, Because the sample contains water, it is difficult to grasp the final volatilization degree of ether, resulting in insufficient extraction of sample components or poor repeatability; (3) ether is a precursor organic solvent, which is harmful to the body of the test personnel: long-term low-concentration inhalation may cause Cause headache, dizziness, fatigue, lethargy, proteinuria, polycythemia and other adverse symptoms

Method used

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  • Thin-layer chromatographic detection method of curcuma zedoary in Fushengkang tablet
  • Thin-layer chromatographic detection method of curcuma zedoary in Fushengkang tablet
  • Thin-layer chromatographic detection method of curcuma zedoary in Fushengkang tablet

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Take 15 tablets of Fushengkang, grind them finely, put them in a round-bottomed flask, add 300ml of water, connect the volatile oil measuring device, add water from the upper end of the measuring device to fill the scale part, and until it overflows into the flask, add 1ml of ethyl acetate, and connect to the condensing oil detector. tube, slowly heated to boiling, kept boiling slightly for 2 hours, allowed to cool, and divided into ethyl acetate solution as the test solution. Another 0.4 g of Curcuma reference drug was taken, and the reference drug solution was prepared in the same way. Take 15 μl of each of the above two solutions, spot them on the same silica gel G thin-layer plate, use petroleum ether (60-90°C)-ethyl acetate-glacial acetic acid (volume ratio 94:5:1) as the developing agent, develop and take out , dried in the air, sprayed with freshly made vanillin test solution, and heated at 105°C until the spots were clearly colored.

[0057] Thin-layer chromato...

Embodiment 2-4

[0059] Preparation of the test solution: take 15 pieces of Fushengkang tablets, grind them finely, put them in a round bottom flask, add 300ml of water, connect the volatile oil measuring device, add water from the upper end of the measuring device to fill the scale part, and when it overflows into the flask, add Ethyl acetate 1ml, connected to a condenser, slowly heated to boiling, kept at a slight boil for 2 hours, allowed to cool, fractionated ethyl acetate solution, as the test solution, sample volume: 15µl.

[0060] Preparation of reference medicinal material solution: Take about 0.4 g of reference medicinal material Curcuma curcuma (Wen Yujin), and prepare a reference medicinal material solution with the same preparation method as the test solution, and the sample volume: 15 µl.

[0061] Thin-layer board: prefabricated silica gel G thin-layer board, specification: 20cm×10cm, Merck Chemical Technology (Shanghai) Co., Ltd. (batch number: HC43300156), Qingdao Ocean Chemical ...

Embodiment 2

[0066] Example 2: Merck board, temperature 24°C, relative humidity 55%.

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Abstract

The invention discloses a thin-layer chromatographic detection method of curcuma in Fushengkang tablets. This method uses ethyl acetate to extract the volatile oil in Fushengkang as the test solution; and uses the same method to process the reference medicinal material Curcuma to make a reference medicinal solution; petroleum ether (60-90°C)-ethyl acetate-glacial acetic acid is used as Developing agent, use silica gel thin-layer plate to develop, spray with newly prepared vanillin test solution, heat at 105°C until the spots are clear in color; If there are no spots, it means that the finished product of Fushengkang contains zedoary ingredients; and if the chromatogram of the test product does not show the main spot of the same color at the position corresponding to the chromatogram of the reference medicinal material, it means that the finished product of Fushengkang does not contain zedoary ingredients. The present invention uses ethyl acetate to reflux heat the sample instead of using ether to sonicate the sample, which solves the problems of sample gelatinization, adhesion, and difficult filtration, and reduces the potential harm to human health; the color development result is accurate: the spots are clear and reproducible Good performance and high accuracy.

Description

technical field [0001] The invention belongs to the technical field of drug detection, in particular to a thin-layer chromatography detection method of curcuma in Fushengkang tablets. Background technique [0002] Fushengkang Tablets are made from the combination of Pukuizi, Xishuguo, Curcuma, Bupleurum, Gynostemma, Shiitake Mushroom, Astragalus and Licorice. Curative effect, curative effect of chemotherapy, and can enhance the immune function of the body and improve the clinical symptoms of patients with liver cancer. As an oral preparation of anti-cancer traditional Chinese medicine, Fushengkang is a pure traditional Chinese medicine anti-malignant drug exclusively produced in the country. It should have a quality detection method with good reproducibility and strong specificity. [0003] The traditional Chinese medicine Curcuma is the dried rhizomes of Zingiberaceae plants, Curcuma Curcumae, Curcuma Curcumae, and Curcuma Curcuma. It was first published in "Medicinal Prop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/90
CPCG01N30/90
Inventor 黄玉秋李珂孙慧慧翟昌梅赵永乐
Owner 青岛华仁太医药业有限公司
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