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Method for detecting components of scutellaria baicalensis

A technology of Scutellaria baicalensis and baicalin, which is applied in the field of detection of components of Scutellaria baicalensis, can solve problems such as inability to complete detection efficiently and quickly, complex mobile phase preparation, and long separation time, and achieve good peak shape, good repeatability and stability, and high resolution high effect

Pending Publication Date: 2022-05-24
BEIJING WEHAND BIO PHARMA CO LTD +1
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Problems solved by technology

Tian Tian et al. carried out ultrasonic extraction of Scutellaria baicalensis medicinal materials, and used HPLC method, C18 chromatographic column, mobile phase was methanol-0.22% phosphoric acid solution, gradient elution, determined baicalin, baicalein, wogonin, and scutellarin A four The content of the three components can be well separated, but the retention time of the last peaked melaleucain A is 65min, and the separation time is longer (Study on HPLC fingerprints of Scutellaria baicalensis from different origins and different years "Zhejiang Agricultural Science", 2018, 59(3))
[0006] At present, most of the reports on the simultaneous determination of baicalin, baicalein, wogonin and scutellarin A use gradient elution, which takes a long time to analyze, or the preparation of mobile phase is complicated, pH needs to be adjusted, and the operation is cumbersome and inefficient. Fast detection

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  • Method for detecting components of scutellaria baicalensis
  • Method for detecting components of scutellaria baicalensis
  • Method for detecting components of scutellaria baicalensis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1, preparation and detection of test substance and reference substance solution

[0039] (1) Preparation of the test solution: Precisely weigh 0.2 g of Scutellaria baicalensis decoction pieces powder (passed through a 20-mesh sieve), put it in a conical flask with a stopper, add 25 mL of methanol aqueous solution with a volume fraction of 70%, weigh it, and ultrasonically treat it for 30 minutes, let it cool to room temperature, add 70% methanol aqueous solution to make up the weight, shake well, filter with a 0.45 μm microporous membrane, and take the filtrate to obtain the test solution.

[0040] (2) Preparation of reference substance solution: Precisely weigh an appropriate amount of each reference substance, add methanol to prepare 1.58975 mg of baicalin reference substance, 54.39 μg of baicalein reference substance, 21.04 μg of wogonin reference substance, and 1 mL of baicalin reference substance. A mixed reference solution of 11.83 μg of reference subst...

Embodiment 2

[0045] Embodiment 2, mobile phase elution ratio investigation

[0046] The test solution and the reference solution were prepared according to the method of Example 1, and injected into high performance liquid chromatography for measurement.

[0047] Chromatographic conditions: Diamonsil C18 (250mm×4.6mm, 5μm) chromatographic column, mobile phase methanol-0.2% phosphoric acid aqueous solution, isocratic elution for 25min, flow rate 1.0ml per minute, column temperature 25°C, detection wavelength 275nm, injection Amount of 10μl.

[0048] Control the elution ratio of the mobile phase (methanol: 0.2% phosphoric acid aqueous solution, v / v) to be 55:45, 65:35, 70:30, and 75:25, respectively, and record the resolution and retention time of the four components. The results are shown in the table. 2-3.

[0049] Table 2 Influence of mobile phase elution ratio on separation effect

[0050]

[0051] Table 3 Retention time of 4 components in the investigation of mobile phase elution ...

Embodiment 3

[0055] Embodiment 3, column temperature investigation

[0056] The test solution and the reference solution were prepared according to the method of Example 1, and injected into high performance liquid chromatography for measurement.

[0057] Chromatographic conditions: Diamonsil C18 (250mm×4.6mm, 5μm) chromatographic column, mobile phase methanol-0.2% phosphoric acid aqueous solution, the volume ratio of methanol and phosphoric acid aqueous solution is 65:35, isocratic elution for 25min, flow rate 1.0ml per minute , the detection wavelength was 275 nm, the injection volume was 10 μl, and the column temperature was controlled to be 20, 25, and 35 °C, respectively, and the resolution and retention time of the four components were recorded. The results are shown in Table 4-5.

[0058] Table 4 The effect of controlling the column temperature at 20, 25, and 35 °C on the separation effect of the four components

[0059]

[0060] Table 5 Retention time of 4 components in column ...

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Abstract

The invention discloses a method for simultaneously detecting baicalin, baicalein, wogonin and oroxylin A in radix scutellariae, which is provided by the invention. The method comprises the following steps: 1) preparing a scutellaria baicalensis sample solution to be detected and a reference substance solution; (2) detecting by adopting a high performance liquid chromatography; chromatographic conditions adopted by the high performance liquid chromatography are as follows: a mobile phase is a mixed solution of methanol and a phosphoric acid aqueous solution with the mass fraction of 0.1%-0.4%, and the volume percentage content of the methanol is 65%-70%; the elution mode is isocratic elution. By adopting the detection method disclosed by the invention, the chromatographic peaks of the baicalein, the baicalin, the wogonin and the oroxylin A can reach baseline separation, and the separation degree is greater than 1.5. According to the method, the organic solvent-phosphoric acid aqueous solution is used as the mobile phase, the elution ratio is fixed, the chromatographic peak shape is good, the separation degree and the accuracy are high, the cost is low, the detection time is shortened, the analysis efficiency is improved, and the consumption of the mobile phase is reduced.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and particularly relates to a method for detecting components of Scutellaria baicalensis. Background technique [0002] Scutellaria baicalensis in traditional Chinese medicine is the dry root of Scutellaria baicalensis Georgi., a labiatae plant, bitter in taste and cold in nature. Cough caused by acute bronchitis and pneumonia. [0003] Flavonoids are the main chemical components and active ingredients in Scutellaria baicalensis, which mainly exist in the form of glycosides or aglycones, of which baicalin has the highest content. The content of baicalin contained in the 2020 edition of the Chinese Pharmacopoeia (Part I) is determined by baicalin. Therefore, the quality control of Scutellaria baicalensis medicinal materials or preparations related to Scutellaria baicalensis is carried out with baicalin as the index. However, in view of the complex components contained in traditional Chines...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/34
CPCG01N30/02G01N30/34G01N2030/027
Inventor 刘志华刘璐冯遇姜丹王玉洁陈路晓刘瑾如王丽邹媛媛
Owner BEIJING WEHAND BIO PHARMA CO LTD
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