Method for detecting purity of pimpinolide

Abstract

The invention discloses a method for detecting the purity of pimpinolide. The invention belongs to the technical field of traditional Chinese medicine purity detection. The method comprises the following steps: (1) preparation of a test solution: precisely weighing 1.75-3.0 mg of a pimpinolide test sample, putting the test sample into a 1mL or 3mL volumetric flask, fixing the volume to a scale byusing a 50% acetonitrile-water mixed solution, uniformly shaking, passing through a 0.22 mu m microfiltration membrane or centrifuging, and taking the supernatant for later use; (2) detecting the testsolution by using ultra-high performance liquid chromatography and gradient elution, wherein the detection conditions are as follows: a chromatographic column is a reversed-phase C18 column; the column temperature of the chromatographic column is 20-45 DEG C; a mobile phase: the mobile phase A is methanol or acetonitrile; the mobile phase B is water; wherein the flow rate is 0.2 mL / min to 0.5 mL / min; the detector is a diode array detector, and the detection wavelength of the diode array detector is 254-330nm; wherein the sample size of the pimpinolide test solution is 0.2 mu L-1. 0mu L. The invention further discloses a detection method of the pimpinolide. The method provided by the invention has the characteristics of accuracy, sensitivity and quickness, provides reliable guarantee for impurity analysis of the pimpinolide, and also saves time and material cost.

Description

technical field [0001] The invention belongs to the technical field of drug purity detection, and in particular relates to a method for detecting the purity of anisolactone. Background technique [0002] Anisolactone, English name: Pimpinellin, chemical name: 5,6—dimethoxy—2H—furo[2,3—h]chromen—2—one, the structural formula is shown in the following formula, and aniselactone belongs to the coumarin class The compound is a light yellow solid, and it is a secondary metabolite of medicinal plants such as limpet, lovage, and angelica. Modern studies have shown that anisolactone has obvious biological activity and can relieve pain (Wang Mengyue, Jia Minru, Ma Yuying, et al. Research on the chemical constituents of the analgesic effective part of Angelica dahurica[J]. Chinese Journal of Pharmaceutical Sciences, 2005(8): 583— 585), hemostasis (Sun Wenbo. Study on the hemostatic active ingredients and mechanism of the blood root bark of Feilong palm [D]. Guizhou Medical University,...

AI Technical Summary

Problems solved by technology

However, the fingerprints of modern medicinal materials related to anisolactone (Wei Qi, Wang Jin, Yu Jin, et al. Comparative study on coumarin compounds in 10 species of bitter bamboo leaves[J]. Journal of China Pharmaceutical University, 2014, 45 (3): 297—300), phytochemical constituents (Song Pingping, Lv Ye, Xu Zenglai, et al. Study on the chemical constituents of the root of Angelica sinensis from Qinghai [J]. Chinese Materia Medica, 2014, 37(1): 55—57), Pharmacology (Sun Wenbo. Research on the hemostatic active ingredients and mechanism of action of the blood root bark of Feilongzhang[D]. Guizhou Medical University, 2018) research has been relatively mature, but the method of purity detection of anisolactone is rarely reported

Anisolactone is derived from plants. Due to the complex chemical composition of phytochemicals, there are many types, and some components have a high degree of similarity. Among them, these chemical components may be prepared together with the target components due to insufficient resolution of high-performance liquid chromatography (HPLC), which may affect their purity

The laboratory needs to build its own method for the detection of the purity of aniselide. At present, the HPLC method is mostly used for detection. However, this method consumes a lot of samples and takes a long time to explore. The separation of compounds with similar properties is not as good as that of ultra-high performance liquid chromatography ( ultra-high performance liquid chromatography), a waste of manpower, material and financial resources

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