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Detection method of gold gall powder

A detection method and technology of gold bile powder, which can be used in measurement devices, instruments, scientific instruments, etc., can solve the problems of low detection sensitivity, low sensitivity and low accuracy, and achieve high detection accuracy, good repeatability and stability. good effect

Pending Publication Date: 2022-04-29
CHONGQING KINBEAR BIOTECHNOLOGY CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Bile acids have the characteristics of weak ultraviolet absorption, or only terminal absorption. When using ultraviolet detectors for detection, low wavelengths should be used for detection; and at the low wavelength end, the response value of bound cholic acids is much higher than that of free forms. The response value of cholic acid substances is large, and various organic solvents interfere with the components to be measured, and there are problems such as baseline fluctuations, large noise, low sensitivity, poor linearity, and low accuracy
[0003] It is known that the main components of bear bile powder (golden bile powder) are tauroursodeoxycholic acid and taurochenodeoxycholic acid, but during the biotransformation process, taurocholic acid, taurin-7-one Cholelithic acid, ursodeoxycholic acid and chenodeoxycholic acid and other impurities
However, the polarity of the bile acids contained in bear bile powder is inconsistent, which makes it difficult to effectively separate the main components and related substances with the same chromatographic system during the detection process.
In the process of reproducing the method of Chinese Pharmacopoeia in 1996 and the method published by Zhao Yong et al. in West China Pharmaceutical Journal, it was found that impurities such as tauroursodeoxycholic acid and taurour-7-ketocholic acid could not be separated, and its detection sensitivity was lower than that of low, and poor detection accuracy

Method used

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  • Detection method of gold gall powder
  • Detection method of gold gall powder
  • Detection method of gold gall powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The present embodiment provides a kind of detection method of cholic acid substance in golden bile powder, and this detection method comprises:

[0038] 1. Instruments and testing conditions

[0039] Chromatographic column: C18 chromatographic column (4.6*250mm, 5μm);

[0040] Injection volume: 10μL;

[0041] Flow rate: 1.5mL / min;

[0042] Column temperature: 30°C;

[0043] Detector: evaporative light detector;

[0044] Drift tube temperature: 45°C;

[0045] Gas flow: 1.5L / min;

[0046] Mobile phase: mobile phase A: 0.3% tetrahydrofuran aqueous solution; mobile phase B: 0.2% trifluoroacetic acid methanol solution;

[0047] Adopt double mobile phase (mobile phase A and mobile phase B) to carry out gradient elution, the condition of gradient elution is as shown in table 1:

[0048] Table 1 gradient elution conditions

[0049] time (min) Mobile phase A(%) Mobile phase B(%) 0 78 2 10 55 45 17 50 50 17.1 78 22 20 78 22 ...

Embodiment 2

[0060] In this example, the linearity and range of tauroursodeoxycholic acid and taurourchenodeoxycholic acid were investigated.

[0061] Take an appropriate amount of tauroursodeoxycholic acid and taurourchenodeoxycholic acid reference substances, and prepare the concentrations of 0.05mg / mL, 0.08mg / mL, 0.10mg / mL, 0.12mg / mL, 0.15mg respectively with diluent / mL of the reference substance mixed solution. Take 10 μL of the solution and inject it into a liquid chromatograph (using the chromatographic conditions of Example 1), and record the chromatogram. The results are shown in Table 2-3.

[0062] Table 2 Tauroursodeoxycholic acid linearity test

[0063] Numbering Injection amount (μg) lg injection volume Peak area lg peak area 1 0.465 -0.333 237.73 2.376 2 0.744 -0.128 504.01 2.702 3 0.930 -0.032 737.91 2.868 4 1.115 0.047 974.02 2.989 5 1.394 0.144 1450.01 3.161

[0064] Table 2 Taurochenodeoxycholic acid linearit...

Embodiment 3

[0068] This example investigates the detection accuracy of tauroursodeoxycholic acid and taurourchenodeoxycholic acid.

[0069] Take an appropriate amount of tauroursodeoxycholic acid and taurourchenodeoxycholic acid reference substances, and prepare the crude concentrations of 80% (about 0.08 mg / mL), 100% (about 0.1 mg / mL), and 120% (about 0.12 mg / mL) respectively. mg / mL), each concentration prepares 3 parts, respectively gets 10 μ L of solution and injects in the liquid chromatograph (using the chromatographic condition of embodiment 1), records the chromatogram, calculates the rate of recovery of impurity, test result is shown in the table 4.

[0070] The recovery rate test result of table 4 tauroursodeoxycholic acid, taurourchenodeoxycholic acid

[0071]

[0072] The results in Table 4 show that: the average recoveries measured by 9 recovered samples at 3 concentration levels are all in the range of 98%-102%, and the RSDs are all less than 2.0%, which meets the require...

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Abstract

The invention belongs to the technical field of chemical drug analysis, and discloses a detection method of gold-gallbladder powder. According to the detection method, high performance liquid chromatography is adopted for detection, and the conditions of the high performance liquid chromatography are as follows: a mobile phase: a mobile phase A: a tetrahydrofuran aqueous solution; and the mobile phase B is a trifluoroacetic acid methanol solution. The detection method can be used for simultaneously detecting six cholic acid substances such as tauroursodeoxycholic acid, taurochenodeoxycholic acid, taurocholic acid, tauro-7-ketocholic acid, ursodeoxycholic acid and chenodeoxycholic acid, has the advantages of high detection accuracy, good repeatability, good stability and the like, and can meet the actual detection requirements of the quality of the golden bile powder.

Description

technical field [0001] The invention belongs to the technical field of chemical drug analysis, and in particular relates to a detection method of golden gallbladder powder. Background technique [0002] Bile acids are usually divided into bound bile acids and free bile acids, among which tauroursodeoxycholic acid and taurochenodeoxycholic acid are bound bile acids, while ursodeoxycholic acid and Chenodeoxycholic acid and the like are free bile acids. Bile acids have the characteristics of weak ultraviolet absorption, or only terminal absorption. When using ultraviolet detectors for detection, low wavelengths should be used for detection; and at the low wavelength end, the response value of bound cholic acids is much higher than that of free forms. The response value of cholic acid substances is large, and various organic solvents interfere with the components to be measured, and there are problems such as baseline fluctuations, large noise, low sensitivity, poor linearity, ...

Claims

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Application Information

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IPC IPC(8): G01N30/34G01N30/04
CPCG01N30/34G01N30/04
Inventor 王海丞李雪梅周健唐宗兴詹付凤曹晖吴孟华
Owner CHONGQING KINBEAR BIOTECHNOLOGY CO LTD
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