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Fingerprint of Cortex Periplocae and quality detection method for Cortex Periplocae

A technology of fingerprints and saponica bark, which is applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of too much loss of reagents, inability to represent the efficacy, toxicity, and adverse reactions of saponica bark

Active Publication Date: 2016-11-23
TIANJIN TASLY PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The original plant of Panspermia barbatus is wild, there is no standardized planting base, and the quality of medicinal materials is difficult to control. The cardiac glycosides contained in it (Saloxin, etc.) are both active ingredients and toxic ingredients. Poisoning is also common
The 2010 edition of "Chinese Pharmacopoeia" only measured the content of 4-methoxy salicylaldehyde, and the index is single, so it is difficult to control the overall quality of Xiangjiapi
Xiangjiapi has a variety of pharmacological effects. In recent years, Xiangjiapi has been used as a traditional Chinese medicine to treat chronic congestive heart failure. However, adverse reactions and fatal cases are often reported in the medication, which is related to its own toxicity.
Although the 2010 edition of the Chinese Pharmacopoeia indicated that the bark bark is poisonous, there is only one index of 4-methoxysalicylaldehyde under the content determination item. This component is the main aroma component of the bark bark and cannot represent the efficacy of the bark bark. and toxicity, so the quality of Persica bark cannot be effectively controlled
Simultaneous determination of the contents of 4-methoxysalicylaldehyde, chlorogenic acid and baricillin in Xiangjia bark has not been reported
At present, only Li Danyi has conducted the HPLC fingerprint research on the fingerprints of Cortex Cyanorrhizae. Most of the research on the chemical components and quality standards of Cortex Cyanorrhizae is the content determination and analysis of a single component as an index. Li Danyi et al. Research on fingerprints, but the detection time of the established HPLC fingerprints is 80 minutes, which takes a long time to analyze and consumes a lot of reagents, which is not conducive to the analysis of multiple batches of samples

Method used

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  • Fingerprint of Cortex Periplocae and quality detection method for Cortex Periplocae
  • Fingerprint of Cortex Periplocae and quality detection method for Cortex Periplocae
  • Fingerprint of Cortex Periplocae and quality detection method for Cortex Periplocae

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0111] (1) Preparation of reference substance solution

[0112] Take appropriate amount of reference substances of chlorogenic acid, 4-methoxysalicylaldehyde, and salicyloxin respectively, weigh them accurately, dissolve them in methanol, and shake them well to make the mass concentrations of 33.24mg L respectively. -1 , 161.1mg·L -1 , 96.80mg·L -1 The stock solution of the mixed reference substance was stored in a refrigerator at 4°C for use. Precisely measure 5mL of the stock solution of the mixed reference substance, put it in a 10mL measuring bottle, add methanol to dilute to the mark, shake well, and use it as a mixed reference solution for content determination. The mass concentration is 16.62mg·L -1 , 8.05mg·L -1 , 4.84mg·L -1 , stored in a 4°C refrigerator for later use.

[0113] (2) preparation of test solution

[0114] Persica persica samples (No. S5 sample in Table 1) were dried and crushed, and 0.25 g of each sample powder (passed through a No. 3 sieve) was ...

Embodiment 2

[0127] (1) Preparation of reference substance solution

[0128] Same as Example 1

[0129] (2) preparation of test solution

[0130]The Persica sinensis sample is No. H6 sample of table 1, and other parts are with embodiment 1.

[0131] (3) Determination and generation of control fingerprints

[0132] Draw and mix reference substance solution and need testing solution (H6), inject ultra-high performance liquid chromatograph, obtain chromatogram, according to chromatogram (see attached Figure 7 ) to calculate the content of the corresponding ingredients in the test product (see Table 8).

[0133] Table 8

[0134]

[0135] The chromatographic conditions are: WATERS ACQUITY UPLC BEH C 18 Chromatographic column (2.1 mm x 100 mm, 1.7 μm). The mobile phase is 0.2% phosphoric acid aqueous solution (A)-methanol (B); the gradient elution program is shown in Table 9. Flow rate 0.4mL·min -1 ; detection wavelength 225nm; column temperature 30°C; injection volume 0.5μL.

[013...

Embodiment 3

[0143] (1) Preparation of reference substance solution

[0144] Same as Example 1

[0145] (2) preparation of test solution

[0146] The Persica sinensis sample is No. H4 sample of table 1, and other parts are with embodiment 1.

[0147] (3) Determination and generation of control fingerprints

[0148] Draw and mix reference substance solution and need testing solution (H4), inject ultra-high performance liquid chromatograph, obtain chromatogram, according to chromatogram (see attached Figure 8 ) to calculate the content of the corresponding ingredients in the test product (see Table 11).

[0149] Table 11

[0150]

[0151]

[0152] The chromatographic conditions are: WATERS ACQUITY UPLC BEH C 18 Chromatographic column (2.1 mm x 100 mm, 1.7 μm). The mobile phase is 0.3% phosphoric acid aqueous solution (A)-methanol (B); the gradient elution program is shown in Table 12. Flow rate 0.4mL·min -1 ; Detection wavelength 225nm; Column temperature 33°C; Injection volum...

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Abstract

The invention relates to a determination method for effective components of Cortex Periplocae. The method is characterized by comprising the following steps: (1) preparation of a control solution: weighing control substances consisting of chlorogenic acid, 4-methoxysalicylaldehyde and periplocin and adding methanol to prepare the mixed control solution; (2) preparation of a test solution: drying and crushing Cortex Periplocae, then sieving the crushed Cortex Periplocae, carrying out precise weighing, adding a methanol solution, then carrying out extraction for 20 to 50 min, carrying out standing for cooling, then carrying out centrifugation and taking supernatant so as to obtain the test solution; and (3) determination: sucking up the mixed control solution and the test solution, injecting the mixed control solution and the test solution into a liquid chromatograph so as to obtain chromatograms and calculating the contents of corresponding components in a test substance according to the chromatogram.

Description

Technical field: [0001] The invention relates to a detection method of traditional Chinese medicine, in particular to a method for establishing the fingerprint of Chinese medicine Persica sinensis and determining the content of related components Background technique: [0002] Periploca sepium Bge. is the dry root bark of Periploca sepium Bge., pungent, bitter, warm; poisonous. Return liver, kidney, heart channel. It has the effects of diuresis, swelling, rheumatism, and strengthening bones. It is also commonly used in the treatment of chronic heart failure in clinical practice. The original plant of Panspermia barbatus is wild, there is no standardized planting base, and the quality of medicinal materials is difficult to control. The cardiac glycosides contained in it (Saloxin, etc.) are both active ingredients and toxic ingredients. Poisoning is also common. The 2010 edition of "Chinese Pharmacopoeia" only measured the content of 4-methoxy salicylaldehyde, which has a s...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 鄂秀辉李丽何毅宋兆辉
Owner TIANJIN TASLY PHARMA CO LTD
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