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Method for Establishing Fingerprint of Xianling Gubao Capsules and Its Quality Detection Method

A technology of Xianlinggubao and fingerprints, applied in the field of quality detection of traditional Chinese medicines, can solve problems such as low quality standards

Active Publication Date: 2017-07-04
GUOYAOJITUAN TONGJITANG (GUIZHOU) PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, so far, the quality standards for Xianling Gubao are relatively low. The current State Food and Drug Administration Drug Standard (Trial) (WS-10269(ZD-0269)-2002) only applies to the single ingredient Epimedium The content of icariin is stipulated, that is, "the content of icariin per gram of Xianling Gubao capsule powder is not less than 3 mg"

Method used

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  • Method for Establishing Fingerprint of Xianling Gubao Capsules and Its Quality Detection Method
  • Method for Establishing Fingerprint of Xianling Gubao Capsules and Its Quality Detection Method
  • Method for Establishing Fingerprint of Xianling Gubao Capsules and Its Quality Detection Method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0083] Embodiment 1 UPLC chromatographic conditions exploration and optimization

[0084] 1. Investigate different chromatographic columns

[0085] Inspected Acquity UPLC BEH Shield RP C18 column (2.1×50mm, 1.7μm), Acquity UPLC BEH Phenyl (2.1×50mm, 1.7μm), Acquity UPLC HS S T3 column (2.1×50mm, 1.8μm), Acquity UPLC BEH Amide (2.1×50mm, 1.7μm) 4 different chromatographic columns, the results are as follows figure 1 shown. Depend on figure 1 It can be seen that the separation effect and the number of chromatographic peaks of the Acquity UPLC BEH Shield RP C18 column are significantly better than other chromatographic columns, so Acquity UPLC BEH Shield RP C18 was selected as the chromatographic column for Xianling Gubao fingerprint analysis.

[0086] 2. Investigate different mobile phase systems

[0087]Investigated ACN-H2O (each containing 0.1% FA), ACN-H2O, MeOH-H2O (each containing 0.1% FA), MeOH-H2O4 different mobile phase systems, the results are as follows figure 2 ...

Embodiment 2

[0100] The pretreatment method investigation of embodiment 2 samples

[0101] 1. Investigate different ratios of extraction solvents

[0102] Take Xianling Gubao Capsules with batch number 1308031, and accurately weigh 8 servings, each serving is about 0.10000g. As shown in Table 1, 8 parts of Xianling Gubao Capsules were placed in 5mL volumetric flasks respectively, and 4mL of extraction solvents (water, 30% methanol-water, 60% methanol-water and methanol) were added in different proportions respectively. Ultrasound (power 150W, frequency 40kHz) for 30min, take it out and let it cool to room temperature to extract the solvent to volume. Shake well and transfer to a 10mL centrifuge tube, centrifuge at 10,000rpm for 1 minute, take the supernatant and pass through a 0.22:μm microporous filter membrane, and continue the filtrate for UPLC analysis. The test pattern is as follows Figure 5 shown.

[0103] Table 1 The investigation of different ratios of extraction solvents

[0...

Embodiment 3

[0114] The preparation of embodiment 3 need testing solution

[0115] Take the content of Xianling Gubao Capsules (Guizhou Tongjitang Pharmaceutical Co., Ltd., batch number 1308031), accurately weigh about 0.10000g, put it in a 5mL volumetric flask, add about 4mL of methanol with a volume fraction of 60%, and ultrasonicate (power 150W , frequency 40kHz) for 30min, take it out, let it cool to room temperature, dilute to 10mL with 60% methanol, so that the concentration of the contents of Xianling Gubao Capsules is 0.02g / mL, shake well, and centrifuge the extract at 10000rpm for 1min. Pass through a 0.22 μm microporous membrane, and take the subsequent filtrate to obtain the test solution of Xianling Gubao Capsules.

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Abstract

The invention provides a method for building a fingerprint spectrum of Xianlinggubao capsules. The fingerprint spectrum of the Xianlinggubao capsules is built by adopting ultrahigh-performance liquid chromatography, and the method comprises the following steps that 1, a test sample solution of the Xianlinggubao capsules is prepared; 2, an epmedin C reference solution is prepared; 3, chromatographic analysis is performed through an ultrahigh-performance liquid chromatograph, and a chromatogram map is recorded; 4, the fingerprint spectrum is obtained according to the relative retention time, obtained through calculation by taking the chromatographic retention time of epmedin C as 1, of all chromatographic peaks, and the chromatographic conditions of the ultrahigh-performance liquid chromatograph are limited. The invention further provides a method for detecting the quality of the Xianlinggubao capsules through the ultrahigh-performance liquid chromatography technology, and detection on the chemical ingredients in the Xianlinggubao capsules is better achieved by adopting different detection wavelengths in different time periods. Compared with existing fingerprint spectrum research on the Xianlinggubao capsule, more characteristic ingredients can be detected; meanwhile, the analysis time is shortened, and solvent consumption is reduced.

Description

technical field [0001] The invention relates to the field of quality detection of traditional Chinese medicines, in particular to a method for establishing a fingerprint of Xianling Gubao capsules, and also relates to a quality detection method for the Xianling Gubao capsules. Background technique [0002] The traditional Chinese medicine compound preparation "Xianling Gubao" Capsule was developed by Professor Shi Guangda, a famous orthopedic expert, based on the bone metabolism balance theory of "kidney governing bone" in traditional Chinese medicine, on the basis of Miao folk prescriptions, and after years of clinical verification and screening. become. It is a compound Chinese patent medicine preparation composed of six traditional Chinese medicines of Epimedium, Dipsacus, Salvia, Psoralen, Anemarrhena, and Rehmannia. Epimedium, also known as fairy spleen, is warm in nature, pungent in taste, sweet, returns to kidney and liver meridian, nourishes kidney essence, and stre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 姚志红戴毅吴肖蒙周先强姚新生周宁
Owner GUOYAOJITUAN TONGJITANG (GUIZHOU) PHARMA CO LTD
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