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Quality monitoring method for quantitative fingerprint spectrum of Shuanghuanglian oral liquid

A technology of Shuanghuanglian oral liquid and fingerprint spectrum, which is applied in the field of compound quality analysis, can solve the problems of difficult to truly reflect the content of caffeoylquinic acids, cumbersome and time-consuming methods, and lack of overall fingerprint control, and achieve a comprehensive analysis method. and the effect of the difference analysis strategy

Inactive Publication Date: 2021-05-28
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

[0005] According to the current Chinese Pharmacopoeia standards, three methods are used to quantitatively determine the main components of the Sanwei prescription in Shuanghuanglian oral liquid, chlorogenic acid, baicalin and forsythin, which are cumbersome and time-consuming
On the other hand, the current standard does not effectively control the overall fingerprint
The simultaneous quantification of 11 components in Shuanghuanglian preparations has been reported in the literature [Bian Tingting. Journal of Pharmaceutical Analysis, 2012,32(1):52-56.; Yang D.Talanta,2011,85(2):885-890.] , which greatly simplifies the detection process, but in order to ensure the accuracy of content determination, it often takes a long analysis time to achieve a better separation effect; at the same time, the quantification of multi-index components greatly increases the difficulty and cost of obtaining reference substances
In addition, the quantitative detection of honeysuckle in Shuanghuanglian oral liquid in the existing literature is mainly aimed at chlorogenic acid, and this component is prone to structural interconversion with neochlorogenic acid and cryptochlorogenic acid [Zhu Peng. ):122-126.], so it is difficult to truly reflect the content of caffeoylquinic acid components

Method used

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  • Quality monitoring method for quantitative fingerprint spectrum of Shuanghuanglian oral liquid
  • Quality monitoring method for quantitative fingerprint spectrum of Shuanghuanglian oral liquid
  • Quality monitoring method for quantitative fingerprint spectrum of Shuanghuanglian oral liquid

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Experimental program
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Effect test

Embodiment approach

[0035] 1. Analysis conditions:

[0036] Instrument: Alliance e2695-2998

[0037] Chromatographic column: Tnature C18 (Acchrom-Tech, 4.6×250mm, 5μm)

[0038] Flow rate: 1mL / min

[0039] Column temperature: 40°C

[0040] Injection volume: 10μL

[0041] Wavelength collection range: 190nm-600nm

[0042] Extraction wavelength: 235nm, 327nm

[0043] Mobile phase: A.0.1% phosphoric acid / acetonitrile (v / v) B.0.1% phosphoric acid / water (v / v)

[0044] gradient:

[0045]

[0046]

[0047] 2. Accurately weigh the reference substance of chlorogenic acid, add water to make a stock solution containing 1000 μg of chlorogenic acid per 1 mL; take the reference substance of forsythin, add 50% methanol / water to make 1000μg stock solution of baicalin; accurately weigh the reference substance of baicalin, add 10% of the total volume of the stock solution with N,N-dimethylformamide to dissolve completely, then add methanol to make a stock solution containing 1000μg of baicalin per 1mL li...

Embodiment 2

[0051] method of execution

[0052] 1. Analysis conditions:

[0053] Instrument: Alliance e2695-2998

[0054] Chromatographic column: Tnature C18 (Acchrom-Tech, 4.6×250mm, 5μm)

[0055] Flow rate: 1.2mL / min

[0056] Column temperature: 40°C

[0057] Injection volume: 10μL

[0058] Wavelength collection range: 190nm-600nm

[0059] Extraction wavelength: 235nm, 327nm

[0060] Mobile phase: A. Volume concentration 0.08% phosphoric acid / acetonitrile B. Volume concentration 0.08% phosphoric acid / water

[0061] gradient:

[0062]

[0063] 2. Mixed standard preparation: with embodiment 1.

[0064] 3. Preparation of test solution: same as in Example 1

[0065] 4. Results: After determination, the test product contained baicalin 14.386mg / mL, forsythin 0.758mg / mL, chlorogenic acid 1.288mg / mL, neochlorogenic acid 0.98mg / mL, cryptochlorogenic acid 0.849mg / mL.

Embodiment 3

[0067] method of execution

[0068] 1. Analytical conditions: with embodiment 1.

[0069] 2. The preparation of need testing solution: with embodiment 1.

[0070] 3. Preparation of mixed standards: 1 mg / mL baicalein, wogonin, wogonin, scutellarin A, chlorogenic acid, isochlorogenic acid A, cryptochlorogenic acid, 3,4-dicaffeoyl Quinic acid, 1,3-dicaffeoylquinic acid, 4,5-dicaffeoylquinic acid, luteolin, rutin, forsythiaside, forsythialin, betulinic acid standard solution, Analyzed directly after filtration through 0.22 μm organic membrane.

[0071] 4. Analysis results: Under the optimal separation conditions, the fingerprint peaks of Shuanghuanglian Oral Liquid were qualitatively analyzed using standard products, and the unknown principal component peaks were qualitatively analyzed by mass spectrometry, as shown in figure 1 , Shuanghuanglian oral liquid contains

[0072] 5. Neochlorogenic acid (3), Secologanoside* (4), chlorogenic acid (5), swertiamarin* (6), cryptochlorog...

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Abstract

The invention relates to a quantitative fingerprint quality monitoring technology for Shuanghuanglian oral liquid, and belongs to the technical field of compound quality analysis. A dual-wavelength quantitative fingerprint spectrum quality control method is established on the basis of a high performance liquid chromatography-ultraviolet detection technology, fingerprint spectrum monitoring of the Shuanghuanglian oral liquid is achieved through one-time analysis, content determination of three index components of chlorogenic acid, baicalin and forsythin is achieved at the same time, and one-standard multi-determination amount of neochlorogenic acid and cryptochlorogenic acid is achieved. According to the method, fingerprint spectrum and quantitative detection are simultaneously realized in one-time analysis, the quality of the Shuanghuanglian oral liquid can be more comprehensively and accurately evaluated, the Shuanghuanglian oral liquid of different manufacturers can be distinguished, meanwhile, the detection time is shortened to the greatest extent, and the resource consumption is reduced.

Description

technical field [0001] The invention relates to a quantitative fingerprint quality monitoring technology of Shuanghuanglian oral liquid, which belongs to the technical field of compound prescription quality analysis. [0002] technical background [0003] Shuanghuanglian Oral Liquid is composed of Scutellaria baicalensis, honeysuckle and forsythia according to the prescription dosage of 1:1:2. Forsythia is the dried fruit of Forsythiasuspensa (Thub.) Vahl, a plant of Oleaceae. It is the main component type, and has the effects of clearing away heat and detoxification, reducing swelling and dispelling stagnation [Xia Wei. Chinese Modern Traditional Chinese Medicine, 2016, 18(12): 1670-1674]; honeysuckle is the dry flower bud or the first bloom of Lonicera japonica Thunb. Scutellaria baicalensis, with chlorogenic acid as the main active substance, is commonly used clinically for antibacterial, antiviral, anti-inflammatory, etc. The dried root of Scutellaria baicalensis Georgi...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/8809
Inventor 梁鑫淼司玮沈爱金刘艳芳金高娃乔亚丽
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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