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Determination method of saffron glycosides in saffron medicinal materials by area normalization method

A technology of crocin and saffron, applied in the field of determination of crocin components in saffron medicinal materials, can solve the problem of inability to quantify the content of total crocin and the inability to fully reflect the true content of total crocin problems, to achieve the effect of solving unstable properties and good repeatability

Active Publication Date: 2019-05-28
HUZHOU CENT HOSPITAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is that "Chinese Pharmacopoeia" only measures the content of crocin-I and crocin-II, which cannot fully reflect the true content of total crocin. Disadvantages of saffron color value cannot quantify the content of total saffron

Method used

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  • Determination method of saffron glycosides in saffron medicinal materials by area normalization method
  • Determination method of saffron glycosides in saffron medicinal materials by area normalization method
  • Determination method of saffron glycosides in saffron medicinal materials by area normalization method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] a. Determine the chromatographic conditions

[0037] Ultimate XB C18 column (250mm×4.6mm, 5μm); column temperature: 30°C; mobile phase: water (A)-methanol (B), gradient elution, 0-60min, B: 20%-100%; DAD Wavelength range 200-600nm, detection wavelength 440nm, flow rate: 1.0mL min -1 ; Injection volume: 10 μL. Under this chromatographic condition, each chromatographic peak has better baseline separation;

[0038] b. Preparation of reference solution

[0039] Precisely weigh 5.96 mg of crocin-I reference substance and 2.96 mg of crocin-II reference substance, put them in a 100 mL brown measuring bottle, dissolve them with dilute ethanol and make up to the mark. The concentration was 59.6μg·mL -1 and 29.6 μg·mL -1 Mix the reference substance solution, shake well, and set aside.

[0040] Crocin-I reference substance solution: Accurately weigh the crocin-Ⅰ reference substance, put it in a brown measuring bottle, dissolve it with dilute ethanol and set the volume to the...

Embodiment 2

[0051] Example 2: Determination of saffron glycosides in 32 batches of saffron medicinal materials at home and abroad

[0052] 1. Instrument

[0053] Agilent 1200 high performance liquid chromatography (Agilent, USA); Agilent 6330 ion trap mass spectrometer, equipped with electrospray ionization source (ESI) (Agilent, USA); Lambda 45 UV-Vis spectrophotometer (PerkinElmer, USA).

[0054] Reagents and Test Articles

[0055] Standard product: Crocin-I (batch number: 111588-201202), crocin-II (batch number: 111589-201304) were purchased from China National Institutes for Food and Drug Control; methanol and formic acid were chromatographically pure (US Tedia company), and the rest of the chemical reagents were of analytical grade.

[0056]Thirty-two batches of saffron medicinal materials were provided by Sandu Saffron Professional Cooperative in Jiande City, Zhejiang Province and different planting bases, and were identified as dried stigmas of Crocus Sativus L. by Professor Chen...

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Abstract

The invention discloses a method for measuring crocin components in stigma croci medicinal materials through an area normalization method. The method comprises the following steps: establishing a stigma croci medicinal material quality control method, separating twelve main crocin components, taking crocin-I which is relatively stable and low in price as an internal reference substance, and measuring the content of the total crocin in the stigma croci medicinal materials by adopting the area normalization method, so that the problems that multiple crocin components cannot be separated when the stigma croci medicinal materials are measured by HPLC (High Performance Liquid Chromatography) and multiple crocin reference substances are difficultly obtained during content measurement are solved. The method comprises the specific steps: taking the crocin-I as the internal reference substance, establishing a relative correction factor of the crocin-I to crocin-II, and calculating the content of the crocin-II; comparing the content of the crocin-I and II in 32 batches of stigma croci measured with an external standard method adopted in the pharmacopeia to validate the feasibility of quantitative analysis of multi-components by single marker. The problem that the crocin-II reference substance is unstable in property and high in price in the pharmacopeia determination method is solved.

Description

technical field [0001] The invention relates to the technical field of analysis of active components of traditional Chinese medicines, in particular to a method for determining saffron glycosides in saffron medicinal materials by combining the one-measurement-multiple-evaluation method and the area normalization method. Background technique [0002] Saffron (Crocus sativus L.), also known as saffron, is only used as medicine with the three red stigmas on the upper part of the pistil. Only 100,000-150,000 flowers can be picked manually to obtain one kilogram of dried saffron. , Cooling blood and detoxification, the effect of relieving depression and calming the nerves. The main active ingredient is crocins, which is a red water-soluble carotene compound. It is a series of ester glycosides formed by combining crocetin with glucose or gentiobiose. It has been isolated and obtained The aglycones are all crocin glycosides of 16 different cis and trans isomers of crocetin. In sa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 钱晓东周桂芬姚冲袁玉梅李丽琴余静芬
Owner HUZHOU CENT HOSPITAL
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