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Method for determining decumbent corydalis tuber total alkaloid extractive content with UFLC and method for establishing UFLC finger print thereof

A technology of total alkaloids and determination methods, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effect of good reproducibility and high precision

Inactive Publication Date: 2010-11-24
SHANGHAI INST OF PHARMA IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Of course, there is no precedent for using UFLC to determine the content of the 6 main alkaloids in summer free total alkaloid extracts

Method used

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  • Method for determining decumbent corydalis tuber total alkaloid extractive content with UFLC and method for establishing UFLC finger print thereof
  • Method for determining decumbent corydalis tuber total alkaloid extractive content with UFLC and method for establishing UFLC finger print thereof
  • Method for determining decumbent corydalis tuber total alkaloid extractive content with UFLC and method for establishing UFLC finger print thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1: UFLC measures the content of alkaloids in summer without total alkaloids extract

[0042] 1 Instruments and reagents

[0043] 1.1 Instrument

[0044] Shimadzu Prominenece UFLC chromatograph (SPD-M20A PDA detector, DGU-20A5 online automatic degasser, LC-20AD pump, SIL-20AC autosampler, CBM-20A diode array detector, CTO-20AC column thermostat) .

[0045] 1.2 Reagent

[0046] Original opioid, palmatine hydrochloride and tetrahydropalmatine standard products were purchased from China Institute for the Control of Pharmaceutical and Biological Products. Standard products of Bikukuling, Charpinine and Corydalis Ermin are self-made with a purity greater than 97%. Methanol is chromatographically pure, glacial acetic acid is analytically pure, distilled water and triethylamine are analytically pure, and summer free medicinal materials are purchased from Yujiang County, Jiangxi.

[0047] Preparation of Corydalis urmin: take 30 g of summer free total alkaloid ext...

Embodiment 2

[0062] Embodiment 2: Establish the UFLC fingerprint spectrum of summer without total alkaloid extract

[0063] Get 10 batches of summer free total alkaloid extracts, according to the assay method identical with embodiment 1, carry out UFLC measurement to 10 batches of extracts, obtain 10 UFLC chromatograms; Compare 10 UFLC chromatograms, determine the common There are 16 characteristic peaks in total. With the retention time and peak area of ​​the chromatographic peak (S peak) of tetrahydropalmatine being 1, the relative retention time and relative peak area of ​​other peaks are calculated to obtain the UFLC without total alkaloid extract in summer Standard Fingerprint. The statistical results of the relative retention time and relative peak area of ​​the common peaks are shown in Table 3 and Table 4, respectively.

[0064] Table 3. Relative retention time statistics (the unit of retention time is min)

[0065] peak number

1

2

3

4

5

6 ...

Embodiment 3

[0069] Embodiment 3: methodological investigation

[0070] 1. Linear analysis of the standard curve of the standard solution

[0071] Draw the standard curve of 6 alkaloid standard solution in embodiment 1, the result is as shown in table 5 below:

[0072] Standard

standard curve line

R 2

cordonine

y=5.077133e -4 X+3.634177

1.0

Tetrahydropalmatine

y=4.123552e -4 X+0.460858

0.9999

Protoopioid

y=3.913227e -4 X+2.171534

0.9999

Violet Ermine

y=3.535232e -4 X-0.1505344

1.0

Palmatine Hydrochloride

y=2.629337e -4 x

0.9999

Bikukuling

y=1.919997e -3 X-0.7133639

1.0

[0073] Among them, e -4 and e -3 Respectively represent "×10 -4 " and "×10 -3 , R stands for linear, R 2 The closer to 1, the better the linearity of the standard curve. As can be seen from the above table, the R of the 6 alkaloid standard solution standard curves 2 Either 1 or infini...

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Abstract

The invention relates to determination of alkaloid content in decumbent corydalis tuber total alkaloid extractive. The determination method comprises the following steps: (1) preparing a decumbent corydalis tuber total alkaloid extractive solution; (2) preparing a standard solution; (3) respectively sucking the extractive solution and the standard solution of an equal amount, and carrying out UFLC determination to obtain a UFLC chromatogram; and (4) analyzing chromatographic peaks of protopine, bicuculline, xiawuning alkaloid, corydaline harmine, tetrahydropalmatine and palmatine in the chromatogram, and calculating contents thereof by an external standard method. Besides, the invention also provides a method for establishing a UFLC finger print of decumbent corydalis tuber total alkaloidextractive. The determination method can quickly and accurately determine contents of six main alkaloids in decumbent corydalis tuber total alkaloid extractive, and the UFLC finger print of decumbentcorydalis tuber total alkaloid extractive can be used for the overall control on substance groups in decumbent corydalis tuber total alkaloid extractive, thereby controlling the quality of extractivefrom the macro analysis perspective.

Description

technical field [0001] The invention relates to a quality control method of summer-free total alkaloid extract and a method for establishing fingerprints. Background technique [0002] The dry tuber or whole plant of Corydalis decumbens (Thunb.) Pers. (C.amabilis Migo), a perennial herb of the genus Corydalis Corydalis in the family Papaveraceae (Papaveraceae) in summer, also known as a golden pill, Wild Yanhu, Immortals in the Cave, Fudi Yanhusuo and Falling Water Drops. Mainly produced in Jiangxi, it is widely distributed in Jiangsu, Anhui, Zhejiang, Fujian, Taiwan, Hunan and other provinces. It is a commonly used Chinese herbal medicine in my country. In summer, it has the effects of promoting blood circulation, dredging collaterals, promoting qi, and relieving pain. It is mainly used to treat stroke and hemiplegia caused by high blood pressure and cerebrovascular diseases, and has good effects on rheumatoid arthritis, sciatica, sequelae of poliomyelitis, etc. Its main ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/86
Inventor 杨义芳张荣劲
Owner SHANGHAI INST OF PHARMA IND
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