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Detecting method of hyoscyamine and hyoscine

A scopolamine and detection method technology, applied in the field of chromatographic analysis, can solve problems such as difficult separation of scopolamine and scopolamine, achieve the effects of shortening the analysis cycle, improving the separation ability, and improving the peak shape

Active Publication Date: 2018-11-30
承德市食品药品检验检测中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problem that scopolamine and scopolamine are difficult to separate in existing prescription preparations, the invention provides a detection method for scopolamine and scopolamine

Method used

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  • Detecting method of hyoscyamine and hyoscine
  • Detecting method of hyoscyamine and hyoscine
  • Detecting method of hyoscyamine and hyoscine

Examples

Experimental program
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Effect test

Embodiment 1

[0044] The embodiment of the present invention provides a detection method for hyoscyamine and scopolamine. The prescription preparation adopts Weitongning Tablets, wherein Weitongning Tablets comprise: 300g of dandelion extract, 300g of aluminum hydroxide, 210g of dried licorice extract, 210g of Tianxianzi extract paste 25g, gentian powder 155g, cumin oil 4mL, and the extract of Tianxianzi contains hyoscyamine and scopolamine.

[0045] The preparation method of the need testing solution of Weitongning tablet is:

[0046] Step a, grind the solid preparation, sample 1.0 g, add 34 times the amount of ethanol with a volume concentration of 75%, ultrasonically extract 3 times, each time for 30 min, centrifuge, combine the supernatant, evaporate to dryness, and obtain the first residue;

[0047] Step b. Dissolve the first residue in an ammonia solution with a mass concentration of 2.16% that is 20 times the sampling mass, add chloroform that is 22 times the sampling mass, perform u...

Embodiment 2

[0070] The embodiment of the present invention provides a detection method for hyoscyamine and scopolamine. The prescription preparation adopts Weitongning Tablets, wherein Weitongning Tablets comprise: 300g of dandelion extract, 300g of aluminum hydroxide, 210g of dried licorice extract, 210g of Tianxianzi extract paste 25g, gentian powder 155g, cumin oil 4mL, and the extract of Tianxianzi contains hyoscyamine and scopolamine.

[0071] The preparation method of the need testing solution of Weitongning tablet is:

[0072] Step a, grind the Weitongning Tablets, sample 1.2g, add 40 times the mass of ethanol with a volume concentration of 70%, ultrasonically extract twice, each time for 35min, centrifuge, combine the supernatant, evaporate to dryness, and obtain the first residue;

[0073] Step b, dissolving the first residue in an ammonia solution with a mass concentration of 2.0% that is 22 times the sampling mass, adding chloroform that is 20 times the sampling mass and perfor...

Embodiment 3

[0091] The embodiment of the present invention provides a detection method for hyoscyamine and scopolamine. The prescription preparation adopts Weitongning Tablets, wherein Weitongning Tablets comprise: 300g of dandelion extract, 300g of aluminum hydroxide, 210g of dried licorice extract, 210g of Tianxianzi extract paste 25g, gentian powder 155g, cumin oil 4mL, and the extract of Tianxianzi contains hyoscyamine and scopolamine.

[0092] The preparation method of the need testing solution of Weitongning tablet is:

[0093] Step a, grind the Weitongning Tablets, sample 0.8g, add 30 times the mass of ethanol with a volume concentration of 80%, ultrasonically extract 3 times, each time for 25min, centrifuge, combine the supernatant, evaporate to dryness, and obtain the first residue;

[0094] Step b, dissolving the first residue in an ammonia solution with a mass concentration of 2.5% that is 17 times the sampling mass, adding chloroform that is 25 times the sampling mass and perf...

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Abstract

The invention relates to the technical field of chromatographic analysis and particularly to a detecting method of hyoscyamine and hyoscine. In the detecting method, HPLC chromatographic analysis is adopted, and the chromatographic conditions are that the chromatographic column is C18 chromatographic column, the flowing phase A is acetonitrile and the flowing phase B is a mixed solution of phosphoric acid and triethylamine. The mass concentration of the phosphoric acid is 0.09-0.11%, the volume concentration of the triethylamine is 0.015-0.025%, the gradient elution sequence is as follows: 0-35 min for the 6% flowing phase A, 35-40 min for the 6%-30% flowing phase A and 40-50 min for the 30%-6% moving phase A; the flowing speed of the flowing phase is 0.9-1.1 mL / min; the detecting wavelength is 210 nm; and the column temperature of the chromatographic column is 34-36 DEG C. The detecting method provided by the invention can detect the peak of the hyoscyamine and the peak of the hyoscine; the peak appearing time is appropriate and the peaks can be well separated from impurity peaks.

Description

technical field [0001] The invention relates to the technical field of chromatographic analysis, in particular to a detection method for scopolamine and scopolamine. Background technique [0002] Hyoscyamine, also known as hyoscine, is one of the belladonna alkaloids isolated from the traditional Chinese medicine Tianxianzi and Dajinhua. Hyoscyamine has the function of relieving pain and spasm, and has a good effect on sciatica. Sometimes it is also used to treat epilepsy and seasickness. [0003] Scopolamine, which is more toxic than anthrax and can be fatal in a slight overdose, is a tropane-type alkaloid that exists in plants of the nightshade family. Scopolamine is an alkaloid with the strongest pharmacological effect in belladonna, which can be used to block parasympathetic nerves, and can also be used as a central nervous system inhibitor. Its hydrobromide is generally used clinically, which can be used for anesthesia, analgesia, It relieves cough and asthma, is effe...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/54
CPCG01N30/02G01N30/06G01N30/54G01N2030/027G01N2030/062
Inventor 马丽杨甲忠王冠蕾孟珊张征
Owner 承德市食品药品检验检测中心
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