Method for simultaneously and quantitatively detecting ligustilide and senkyunolide A

A technology for ligustilide and ligustilide, which is applied in the field of simultaneous quantitative detection of ligustilide and ligustilide A, and can solve the problems of quantitative detection, poor stability of pure products and the like

Active Publication Date: 2014-10-08
SICHUAN ACAD OF CHINESE MEDICINE SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In view of the above situation, the present invention provides a kind of butylphthalide as a substitute reference substance, and adopts high performance liquid chromatography (HPLC) to simultaneously detect ligustilide and cyanide Ligustilide A is carried out the method for quantitative detection, to solve the problem that the pure product of ligustilide and ligustilide A have poor stability and cannot be used as the reference substance for national legal content determination to carry out quantitative detection, realize the detection of ligustilide containing And / or the quantitative detection and monitoring of Liguscaractone A component drugs to ensure the quality of drugs

Method used

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  • Method for simultaneously and quantitatively detecting ligustilide and senkyunolide A
  • Method for simultaneously and quantitatively detecting ligustilide and senkyunolide A
  • Method for simultaneously and quantitatively detecting ligustilide and senkyunolide A

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Quantitative detection of ligustilide and ligustilide A in Chuanxiong:

[0029] According to the high-performance liquid chromatography specified in Appendix VI D of the Chinese Pharmacopoeia 2010 edition.

[0030] 1.1 Chromatographic conditions and system suitability test

[0031] Column: Agilent Eclipse XDB-C 18 (4.6mm×150mm, 5μm); mobile phase: methanol-water (50 : 50); the flow rate is 1.0ml / min; the column temperature is 35°C, and the detection wavelength is 280nm; the number of theoretical plates should not be less than 3000 based on the peak of ligustilide.

[0032] 1.2 Preparation of solution

[0033]1.2.1 Reference substance solution Accurately weigh 49.85 mg of butylphthalide reference substance, put it in a 25ml measuring bottle, add absolute ethanol to dissolve it and adjust the volume to the mark, and shake well to obtain the butylphthalide reference substance stock solution; precisely weigh Put 22.54mg of ligustilide reference substance into a 25ml b...

Embodiment 2

[0080] Quantitative detection of ligustilide and ligustilide A in Angelica sinensis:

[0081] Determined according to high performance liquid chromatography (Appendix VI D of Chinese Pharmacopoeia 2010 Edition).

[0082] 2.1 Chromatographic conditions and system suitability test

[0083] Octadecylsilane bonded silica gel as filler; methanol-water (30 :70) is the mobile phase; the flow rate is 1.5ml / min; the column temperature is 40°C, and the detection wavelength is 280nm; the number of theoretical plates should not be less than 3000 based on the ligustilide peak.

[0084] 2.2 Preparation of solution

[0085] The preparation of reference substance solution and need testing solution is the same as in Example 1.

[0086] 2.3 Linear relationship inspection

[0087] Precisely draw 1, 2, 5, 10, 15, and 20 μl of the above-mentioned mixed reference solution, and measure the peak areas of butylphthalide, ligustilide A, and ligustilide respectively according to 1.1 chromatographi...

Embodiment 3

[0106] Quantitative detection of ligustilide and ligustilide A in Chuanxiong:

[0107] Determined according to high performance liquid chromatography (Appendix VI D of Chinese Pharmacopoeia 2010 Edition).

[0108] 3.1 Chromatographic conditions and system suitability test

[0109] Octadecylsilane bonded silica gel as filler; methanol-water (70 : 30) is the mobile phase; the flow rate is 0.6ml / min; the column temperature is 15°C, and the detection wavelength is 275nm; the number of theoretical plates should not be less than 3000 based on the ligustilide peak.

[0110] 3.2 Preparation of solution

[0111] The preparation of reference substance solution and need testing solution is the same as in Example 1.

[0112] 3.3 Linear relationship inspection

[0113] Precisely draw 1, 2, 5, 10, 15, and 20 μl of the above-mentioned mixed reference solution, and measure the peak areas of butylphthalide, ligustilide A, and ligustilide respectively according to 3.1 chromatographic cond...

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Abstract

The invention discloses a method for simultaneously and quantitatively detecting ligustilide and senkyunolide A. The method comprises the following steps: according to an HPLC (high performance liquid chromatography) method in which butylphthalide serves as a substitution reference substance and octadecyl silane bonded silica gel serves as a filling agent, respectively determining the peak area Ax and the peak area Ay of the ligustilide (X) and the senkyunolide A (Y) in a to-be-detected sample by using a single wavelength in a range of 275-284nm; and according to the concentration Cz and the peak area Az of the substitution reference substance, namely the butylphthalide (Z), calculating the concentration C of the detected components, namely the ligustilide and the senkyunolide A, according to a formula by using correction factors f, wherein a correction factor fx is within 0.20-0.25, and a correction factor fy is within 0.46-0.54. A detection result obtained by using the method provided by the invention is stable, and is in accordance with a detection result obtained by using a method in which the ligustilide and the senkyunolide A, freshly prepared, serve as reference substances, and the problems that the dual-wavelength detection needs to be simultaneously adopted, the requirements on HPLC equipment are high and the universality is poor in the prior art are solved.

Description

technical field [0001] The invention relates to a simple method for quantitatively detecting ligustilide and ligustilide A simultaneously by substituting a reference substance. Background technique [0002] Reference substances are the key to drug quality evaluation and supervision and inspection. In actual work, because some reference substances are expensive, the inspection cost is high, and some reference substances cannot be provided due to instability, which affects the determination of the drug content, making it difficult to control the quality of the drug, which affects the quality of the drug. An important factor in the evaluation and supervision inspection. [0003] Ligustilide and Ligustilide A are the main active ingredients of volatile oils in commonly used traditional Chinese medicines such as Angelica and Chuanxiong. Due to their poor stability, the pure products of ligustilide and ligustilide A cannot be used as reference substances for national legal cont...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 易进海刘云华杨艳刘玉红黄志芳陈燕杨昌林
Owner SICHUAN ACAD OF CHINESE MEDICINE SCI
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