Method for detecting amino acid component in Xiasangju preparation

A technology of amino acids and mulberry chrysanthemum, which is applied in the preparation of test samples, measuring device, material separation, etc., can solve the problem of difficulty in comprehensively characterizing the physical and chemical characteristics of compound mulberry chrysanthemum preparations.

Active Publication Date: 2006-11-22
GUANGZHOU XINGQUN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] All of the above are methods for identification or content determination of individual components, and it is difficult to fully characterize the physical and ch

Method used

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  • Method for detecting amino acid component in Xiasangju preparation
  • Method for detecting amino acid component in Xiasangju preparation
  • Method for detecting amino acid component in Xiasangju preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Example 1 Detection of fingerprints of amino acid components in Xiasangju sugar-containing granules

[0056] 1. Instruments and reagents

[0057] 1.1 Instruments Waters2695 high performance liquid chromatography, Waters 2475 (fluorescence detector), Empower chromatography workstation. Swiss Mettler company AE-200 electronic analytical balance.

[0058] 1.2 Reagent Derivative agent: 6-amino acid quinoline-N-hydroxysuccinimidyl-carbamate (abbreviated as AQC), amino acid reference substance: AminoAcid stadard H (Waters Company); acetonitrile (chromatographically pure), secondary heavy Distilled water, sodium acetate (analytical pure), triethylamine (analytical pure)

[0059] 2. High performance liquid chromatography

[0060]

mobile phase

time

flow

mL.min -1

A

Sodium acetate buffer mL

B

Acetonitrile solution mL

1

2

0

0.5

1

1

100

100

0

0

3

1

1

...

Embodiment 2

[0066] Example 2 Detection of fingerprints of amino acid components in 10 batches of Xiasangju sugar-containing granules

[0067] Get 10 batches of Xia Sangju granules, detect according to the conditions of Example 1, and obtain the amino acid HPLC collection of samples of 10 batches of samples, as figure 2 As shown, by comparing 10 batches of HPLC chromatograms, the similarity evaluation is carried out to determine its characteristic common peak:

[0068] There are 12 common peaks in the fingerprint spectrum. Now the retention time of the spectrum, the average value of the peak area and the RSD value are summarized, as follows:

[0069] Peak No. 1 is aspartic acid, the average retention time RT is 19.54min, the RSD is 0.05%, the peak area is 785808, the RSD is 25.04%, accounting for 1.58% of the total peak area.

[0070] The No. 2 peak is serine, the average retention time RT is 20.45min, the RSD is 0.05%, the peak area is 721818, the RSD is 33.86%, accounting for 1.46% of ...

Embodiment 3

[0088] Example 3 Method for Determination of Fingerprint of Amino Acid Components of Guangzhou Xingqun Xia Sangju Sugar-Containing Granules

[0089] (b) Preparation of the test solution: Accurately weigh 1.0 g of Xia Sangju granules produced by Guangzhou Xingqun (Pharmaceutical) Co., Ltd., put in a 10mL volumetric flask, add water to dissolve to the mark, shake well, and filter with an ultra-microporous membrane , take 10uL filtrate to the derivation tube, add 170uL boric acid buffer, and add 20uL concentration of 0.5% 6-aminoquinolyl-N-hydroxysuccinimidyl-carbamate in acetonitrile solution, vortex mix for 15 In seconds, the sample tube is sealed, placed in a 50°C oven, heated for 20 minutes, and then allowed to cool.

[0090](c) Chromatographic conditions: the chromatographic column is octadecylsilane bonded silica gel as a filler; gradient elution is adopted, and the mobile phase is a mixture of 0.05mol / L sodium acetate buffer (phase A) with a pH of 5.05 and 60% acetonitrile...

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Abstract

The related detection method for amino acid content in Xiasangju preparation comprises: (a) preparing reference solution; (b) preparing sample solution; (c) chromatogram condition: using octadecylsilicane chemically bonded silica as filler, using the gradient elution liquid with 0.05~0.10mol/L NaAc solution buffer and 20-80% acetonitrile solution as mobile phase with pH value as 4.50-5.05, 30-50Deg temperature, activation wavelength 250nm, emission wavelength 395nm, flow rate as 0.5-1.5mL .min-1, and 30-80min; (d) obtaining the fingerprint spectrum with HPLC. This invention is simple and stable, and has well repeatability and precision.

Description

technical field [0001] The invention relates to a quality control method of traditional Chinese medicine preparations, in particular to a method for establishing fingerprints by using high-performance liquid chromatography to detect amino acid components in Xiasangju preparations. Background technique [0002] Xiasangju preparation is a well-known product approved by the state for marketing. It is made of Chinese medicinal materials Prunella vulgaris, mulberry leaves, and wild chrysanthemum. Cold, conjunctival congestion, headache, high blood pressure, dizziness, tinnitus, sore throat, treatment of sores and swollen toxins. Xiasangju preparation has been recorded in the fifteenth volume of Chinese medicine prescription preparations of the Ministry of Health of the People's Republic of China. It is a popular traditional Chinese medicine preparation. Now there are Xiasangju sugar-free granules, Xiasangju oral liquid, Xiasangju beverage and other dosage f...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N1/28G01N30/06G01N30/34G01N30/86
Inventor 孙维广柯雪红苏广丰姚江雄方铁铮
Owner GUANGZHOU XINGQUN PHARMA
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