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Method for simultaneously detecting content of seven ingredients in stomach-benefiting capsules

A Liwei Capsule and Content Technology, which is applied to measurement devices, material separation, analysis of materials, etc., can solve the problems of large differences in physical and chemical properties of chemical components, inability to detect chemical component content, and complex prescription composition, and achieves high peak area, Accurate and fast effects

Active Publication Date: 2019-11-19
JIANMIN PHARMA GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the more complex composition of the prescription in Liwei Capsules, the background interference is very serious, and the physical and chemical properties of the chemical components in Rhubarb and Panax notoginseng are very different, the method in the Pharmacopoeia cannot be used to detect the content of more chemical components in Liwei Capsules at the same time

Method used

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  • Method for simultaneously detecting content of seven ingredients in stomach-benefiting capsules
  • Method for simultaneously detecting content of seven ingredients in stomach-benefiting capsules
  • Method for simultaneously detecting content of seven ingredients in stomach-benefiting capsules

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The selection of embodiment 1 sample preparation method

[0023] Method 1: Take the contents of the capsule, mix well, take about 1.0g, accurately weigh it, put it in a stoppered Erlenmeyer flask, add 50ml of methanol precisely, seal it tightly, weigh it, and ultrasonically treat it (power 250W, frequency 40kHz) for 30 Minutes, let cool, then weigh again, make up the lost weight with methanol, shake well, filter, accurately take 10ml of the filtrate in a conical flask, add 5ml of 2.5mol / l sodium hydroxide, and heat in a water bath at 80°C After 30 minutes, let it cool, add 2.5mol / l hydrochloric acid to adjust the pH value to 2~3, shake and extract twice with ethyl acetate, 10ml each time, combine the ethyl acetate solution, recover the solvent under reduced pressure to dryness, and transfer the residue to In a 10ml measuring bottle, add methanol to the mark, shake well, filter, and take the filtrate to obtain the final product.

[0024] Method 2: Take the contents of t...

Embodiment 2

[0031] The selection of embodiment 2 wavelength

[0032] Sample solution preparation method: the same as method 1 in Example 1.

[0033] Detection wavelength: 210nm, 230nm, 254nm

[0034] Other conditions are identical with embodiment 1.

[0035] result: image 3 is the chromatogram of the detection wavelength of 210nm, and figure 1 In comparison, not only are few components detected, but the area of ​​each peak is less than figure 1 . Figure 4 It is the chromatogram of the detection wavelength of 254nm. It can be seen from the figure that there is no notoginseng saponin R in about 18 minutes 1 Chromatographic peak, ginsenoside Rg around 44 minutes 1 Chromatographic peak areas are much lower than figure 1 Ginsenoside Rg 1 of the peak area. Therefore 230nm is the optimum detection wavelength of the present invention.

Embodiment 3

[0036] Embodiment 3 mobile phase selection

[0037] Sample solution preparation method: the same as method 1 in Example 1.

[0038] Mobile phase 1: 5% tetrahydrofuran acetonitrile solution as mobile phase A, 0.1% phosphoric acid aqueous solution as mobile phase B

[0039] Mobile phase 2: Acetonitrile solution is mobile phase A, water is mobile phase B

[0040] Mobile phase 3: methanol solution is mobile phase A, 0.1% phosphoric acid solution is mobile phase B

[0041] Other conditions are identical with embodiment 1.

[0042] result: Figure 5It is the chromatogram after gradient elution of mobile phase 2, as can be seen from the figure, the mobile phase peak resolution and peak shape without tetrahydrofuran and phosphoric acid are obviously poor, wherein ginsenoside Rg 1 The chromatographic peaks and adjacent peaks are not completely separated, and aloe-emodin is not completely separated from adjacent peaks. Figure 6 It is the chromatogram after adopting mobile phase 3 ...

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Abstract

The invention discloses a method for simultaneously detecting content of seven ingredients in stomach-benefiting capsules. The seven ingredients are ginsenoside Rg1, notoginsenoside R1, aloe-emodin, rhein, rheum emodin, chrysophanol and emodin monomethyl ether. The method comprises the steps of: carrying out ultrasonic extraction on a to-be-detected sample with methyl alcohol; after adding alkaliinto extracting solution to perform a reaction, regulating to pH of 2 to 3 with acid; and finally, extracting with ethyl acetate, and after making up to the volume with methyl alcohol, loading the obtained product onto a high performance liquid chromatographic instrument to carry out detection. According to the invention, the content of seven substances in the stomach-benefiting capsules can be simultaneously detected out, so that quality of a medicine can be more comprehensively represented and controlled, the fake and shoddy phenomena of traditional Chinese medicine are prevented, and the medicine curative effect and medicine use safety are ensured better.

Description

technical field [0001] The invention relates to a method for determining the content of Liwei capsules, belonging to the field of drug analysis. Background technique [0002] CN 1879711A discloses a traditional Chinese medicine composition for treating stomach diseases and its quality control method. The trade name of the Chinese medicine is Liwei Capsules, in which TLC scanning method is used to detect the active ingredients of Panax notoginseng, ginsenoside Rg 1 Carry out the content determination, the notoginseng medicinal material, rhubarb medicinal material, ginsenoside Rg 1 , notoginsenoside R 1 The thin layer identification was carried out, and the physical and chemical properties of the product were also identified, so as to control the quality of the product through qualitative and quantitative detection. [0003] However, the thin-layer scanning method has shortcomings such as large errors, poor reproducibility, and low accuracy. TLC and physical and chemical ide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 吴木琴李霞赵刚陈鹏熊登科向阳朱立彬
Owner JIANMIN PHARMA GRP CO LTD
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