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Detecting method ofgross saponins of tribulusterrestris capsule featurespectrum

A detection method and a characteristic spectrum technology are applied in the field of detection of the characteristic spectrum of Tribulus saponin capsules, which can solve the problems of poor repeatability, low accuracy, and unstable chromatographic baseline of test results, and achieve good separation, high precision, and guaranteed quality effect

Pending Publication Date: 2019-07-12
李梓嘉
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Therefore, the technical problem to be solved by the present invention is to overcome the defects that the chromatographic baseline is unstable in the liquid chromatography method of the characteristic map of Tribulus saponin capsules in the prior art, which leads to poor repeatability and low accuracy of the detection results, thereby providing a kind of Tribulus terrestris saponin Detection method of capsule characteristic map

Method used

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  • Detecting method ofgross saponins of tribulusterrestris capsule featurespectrum

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Experimental program
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Embodiment

[0056] This embodiment provides a method for detecting the characteristic spectrum of Tribulus terrestris capsules, comprising the following steps:

[0057] (1) Determine the liquid chromatography conditions:

[0058] Chromatographic column: Octadecylsilane bonded silica gel as filler, particle size of filler is 5μm, 250mm×4.6mm, column temperature: 30°C;

[0059] Mobile phase: mobile phase A is acetonitrile, mobile phase B is 0.1% formic acid / water mixed solution, the flow rate is 1.0mL / min, gradient elution is adopted, and the gradient elution procedure is shown in Table 1 below:

[0060] Table 1 Mobile phase gradient elution program

[0061] time (minutes) Mobile phase A(%) Mobile phase B(%) 0～18 15→22 85→78 18～55 22→27 78→73 55～62 27→32 73→68 62～80 32→40 68→60 80～90 40→80 60→20

[0062] Injection volume: 10μL;

[0063] Evaporative light scattering detector: the drift tube temperature is 108°C, and the carrier gas flow rate...

experiment example 1

[0083] Experimental Example 1 Specificity Investigation Test

[0084] Get Tribulus Terrestris Capsules (batch number 05180307) and corresponding auxiliary materials (according to the finished product prescription ratio of Tribulus Terrestris Capsules), prepare respectively the test solution, auxiliary material solution and mixed reference solution according to the method of Example 1 of the present invention, wherein:

[0085] The preparation process of the auxiliary material solution is as follows: take 16 mg of auxiliary material, accurately weigh it, place it in a stoppered Erlenmeyer flask, accurately add 10 mL of 50% methanol / water mixed solution, seal it tightly, and weigh it; ultrasonic treatment for 20 minutes (power 900W, frequency 60kHz), cooled to room temperature, weighed again, and made up the lost weight with 50% methanol / water mixed solution; shake well, pass through 0.45μm filter membrane, take the filtrate, and obtain.

[0086] The preparation process of mixed...

experiment example 2

[0089] Experimental Example 2 Precision Inspection Test

[0090] Take Tribulus terrestris saponin capsules (batch number 05180307), prepare the test solution according to the method of Example 1 of the present invention, and carry out liquid chromatography detection according to the chromatographic conditions in Example 1. Continuously inject 5 times, 10 μL each time, record the chromatogram, see Figure 4 As shown, the chromatograms in the chromatogram record correspond to the samples of the 1st, 2nd, 3rd, 4th and 5th injections from bottom to top. The resulting characteristic peak is calculated as peak 5 (S peak), and the relative retention time and relative peak area are shown in Tables 3 and 4 below, respectively.

[0091] Table 3 Inspection of precision—relative retention time of characteristic peaks

[0092] sample injection peak 1 peak 2 peak 3 peak 4 peak 5 Peak 6 Peak 7 1 0.242 0.346 0.426 0.439 1.000 1.041 1.648 2 0.245 0.35...

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Abstract

The invention relates to the technical field of traditional Chinese medicine detection, and discloses a detecting method ofgross saponins of tribulusterrestris capsule featurespectrum.By using an acetonitrile-0.1% of formic acid / water mixed solution as a mobile phase, a gross saponins of tribulusterrestris capsule featurespectrumis obtained by a detecting method adopting gradient elution and combing a liquid chromatogram analysis technique detecting with an evaporative light scattering detector;under the specific detection condition of the detecting method ofthe gross saponins of tribulusterrestris capsule featurespectrum, the obtained chromatographic peak of the gross saponins of tribulusterrestris capsule is uniformly distributed,the resolution of the gross saponins of tribulusterrestriscapsule K reference peak and an adjacent peak is good, and the chromatographic peak information is complete. The detecting method ofthe gross saponins of tribulusterrestris capsule featurespectrum has the characteristics of being simple in operation, stable, reliable, high in precision, high in specificity, and good inresolution.

Description

technical field [0001] The invention relates to the technical field of traditional Chinese medicine detection, in particular to a method for detecting the characteristic spectrum of Tribulus terrestris capsules. Background technique [0002] Tribulus terrestris (Tribulus terrestris L.), also known as white terrestris, thorn terrestris, hard terrestris, Quren, etc., is the dry mature fruit of Tribulus terrestris L., a plant of the family Tribulus terrestris. The research on the chemical composition of Tribulus terrestris began in the 1960s, and it has been confirmed that Tribulus terrestris mainly contains saponins, flavonoids, alkaloids, polysaccharides and other compounds, as well as sterols, amino acids, terpenes, fatty acids, inorganic salts and other components. Modern pharmacological studies have shown that steroidal saponins have a good improvement effect on various diseases such as low immunity and cardiovascular diseases, and can also inhibit the growth of tumor cell...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88
Inventor 翁红王波张子安蔡利剑铁芳
Owner 李梓嘉
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