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Method for determining specnuezhenide content through high performance liquid chromatography

A technology of high performance liquid chromatography and privetin, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of incomplete extraction of privetin and inaccurate analysis, and achieve high sensitivity, good specificity, The effect of optimizing detection conditions

Inactive Publication Date: 2018-09-28
国珍健康科技(北京)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, there are many methods for determining privetin in Ligustrum lucidum by high performance liquid chromatography, but there are problems that the extraction of privetin is not thorough and the analysis is not accurate enough. Based on this, the application proposes a A new method for the content of privetin

Method used

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  • Method for determining specnuezhenide content through high performance liquid chromatography
  • Method for determining specnuezhenide content through high performance liquid chromatography
  • Method for determining specnuezhenide content through high performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The present embodiment relates to the detection method of privet privet glycosides, comprising the following steps:

[0038] A, prepare the standard curve of teruzhenin content

[0039] 1) Precisely pipette 5 μL, 10 μL, 20 μL, 50 μL and 100 μL of 1000 μg / mL tervitalin standard solution, place them in 10 mL colorimetric tubes respectively, dilute to the mark with methanol, and shake well. Gradient standard solutions with concentrations of 0.5 μg / mL, 1 μg / mL, 2 μg / mL, 5 μg / mL and 10 μg / mL were obtained.

[0040] 2) Choose a reversed-phase C18 chromatographic column, the mobile phase is methanol and water with a volume ratio of 35:65, and the flow rate is controlled at 1mL min-1; the column temperature is 35°C, the detection wavelength is 224nm, and the detector is UV-DAD detection device for measurement. Take the standard solution concentration C (μg / mL) as the abscissa, and take the peak area F as the ordinate to plot ( figure 1 ), the resulting linear regression equa...

experiment example 1

[0049] This experimental example involves the verification of the specificity of the method of the present invention, including the following steps: select the same detection conditions as in Example 1, measure the standard solution and sample of 2.0 μg / mL respectively, and compare the privet privet at 15.8min For the spectral lines of glycosides, see figure 2 . by HPLC Figure 7 It shows that the impurity in the sample is well separated from the privetin, and the retention time of the sample is almost the same as that of the privetin in the standard solution, and the method has good specificity.

Embodiment 2

[0051] This experimental example relates to the precision test of the method of the present invention:

[0052] 1) Instrument precision

[0053] Under the same conditions as in Example 1, three standard solutions with a concentration of 2.0 μg / mL were measured in parallel, and the results are shown in Table 1.

[0054] Table 2 Instrument precision (n=3)

[0055]

[0056] It can be seen from Table 1 that the relative standard deviation RSD is 1.43%, and the precision of the test method meets the requirements.

[0057] 2) Method precision

[0058] When using the method "3.1 Sample processing method" to process the sample, three samples of 0.1000g were weighed respectively, and the precision was calculated. The measurement results are shown in Table 2.

[0059] Table 3 method precision

[0060]

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Abstract

The invention relates to a method for determining specnuezhenide content through high performance liquid chromatography. The method comprises the following steps: 1) extracting specnuezhenide from a to-be-tested sample powder containing specnuezhenide with an aqueous solution of methanol having a volume fraction of 55-65% so as to obtain a to-be-tested solution; 2) introducing the to-be-tested solution into a high performance liquid chromatograph, adopting a reversed phase C18 chromatographic column, and taking methanol and water having a volume ratio of 35 to 65 as a mobile phase for detection. According to the method disclosed by the invention, by researching and optimizing the type, the concentration and the solid-liquid ratio of the extracting solution, the specnuezhenide in the samplecan be extracted to the greatest degree under the condition that the extracting solution is not wasted, and a foundation is laid for accurate determination. According to the method disclosed by the invention, the detection conditions of liquid chromatography are further optimized, the methanol and water having a specific ratio is selected as the mobile phase, and the detection accuracy can be effectively improved. The method for determining the specnuezhenide content through high performance liquid chromatography disclosed by the invention has the advantages of being excellent in specificity,high in sensitivity and the like.

Description

technical field [0001] The invention relates to the field of analysis of effective components of traditional Chinese medicines, in particular to a method for determining the content of privet privet in privet lucidum by high performance liquid chromatography. Background technique [0002] Ligustrum lucidi (FructusLigustriLucidi) is the dry mature fruit of the evergreen tree Ligustrum lucidum Ait. in Oleaceae. Initially recorded in "Shen Nong's Materia Medica", the top grade is a medicine for strengthening the body. It is sweet and bitter in taste, cool in nature, and belongs to the liver and kidney meridian. It has the effect of nourishing liver and kidney and improving eyesight and black hair. It is used to treat liver and kidney yin deficiency, dizziness and tinnitus, soreness of waist and knees, premature graying of beard and hair, dark eyes, internal heat and thirst , Bone steaming and hot flashes embolism. Because of its functions of protecting the liver, lowering blo...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 李永强黄瑛陈超温霖李颖李爱民
Owner 国珍健康科技(北京)有限公司
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