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A kind of supercritical chromatographic analysis method of macamides

A technology of supercritical chromatography and macamide, which is applied in the analysis of materials, material separation, instruments, etc., can solve the problems of few research reports, and achieve the effect of solving limitations, fast analysis speed and conditions

Active Publication Date: 2019-03-29
SUN YAT SEN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since 2000, 22 kinds of macamides have been isolated and identified, but there are few research reports on the analysis and detection of the effective components of macamides

Method used

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  • A kind of supercritical chromatographic analysis method of macamides
  • A kind of supercritical chromatographic analysis method of macamides
  • A kind of supercritical chromatographic analysis method of macamides

Examples

Experimental program
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Effect test

Embodiment 1

[0025] A supercritical chromatographic analysis method of macamide components, comprising the following steps:

[0026] (1) Sample preparation: samples include N-benzylhexadecanamide (macamide B) standard and N-(3-methoxy-benzyl)-(9Z,12Z)-octadecadienamide Standard product, using methanol to prepare a mixed standard solution;

[0027] (2) Preparation: Open the CO 2 Gas valve, start the supercritical chromatography system, wait for the pressure of the back pressure valve and the cooling temperature to reach the set value, set the temperature of the chromatographic column to 40°C, the pressure of the back pressure valve to 10MPa, and the flow rate of the mobile phase to 2-5mL / min , the mobile phase was supercritical CO 2 -Modifier, the modifier is dehydrated alcohol, relative to the flow rate of mobile phase, the ratio of dehydrated alcohol is 3%~8%;

[0028] (3) Sample injection: inject the sample liquid prepared in step (1) into the supercritical chromatographic system, and...

Embodiment 2

[0032] A supercritical chromatographic analysis method of macamide components, comprising the following steps:

[0033] (1) Sample preparation: samples include N-benzylhexadecanamide (macamide B) standard and N-(3-methoxy-benzyl)-(9Z,12Z)-octadecadienamide Standard product, using methanol to prepare a mixed standard solution;

[0034] (2) Preparation: Open the CO 2 Gas valve, start the supercritical chromatography system, wait for the pressure of the back pressure valve and the cooling temperature to reach the set value, set the temperature of the chromatographic column to 40°C, the pressure of the back pressure valve to 10MPa, and the flow rate of the mobile phase to 3mL / min, flow The phase is supercritical CO 2 -Modifier, the modifier is absolute ethanol, relative to the flow rate of the mobile phase, the ratio of absolute ethanol is 3.4%, that is, the flow rate of absolute ethanol is 1.02mL / min;

[0035] (3) Sample injection: inject the sample injection liquid prepared i...

Embodiment 3

[0038] Resolution is also called resolution. In order to judge the separation of separated substances in the chromatographic column, the resolution is often used as the total separation performance index of the column. The higher the degree of separation, the better the separation of substances. The degree of separation is represented by R, and R is equal to the ratio of the difference between the retention times of adjacent chromatographic peaks and the average value of the peak width of the two chromatographic peaks, and its calculation formula is: R=2(t R2 -t R1 ) / (W 1 +W 2 ). Among them, t R2 : the retention time of the latter peak among the two adjacent peaks; t R1 : the retention time of the previous peak among the two adjacent peaks; W 1 , W 2 : The peak width of the two adjacent peaks.

[0039] The number of theoretical plates is referred to as the column efficiency, which depends on the type and nature of the stationary phase (particle size, particle size dist...

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Abstract

The invention relates to a supercritical chromatographic analysis method of macamides components. The supercritical chromatographic analysis method comprises the first step of sample preparing, the second step of work preparing, the third step of sample introducing, and the fourth step of detection and analysis. A macamide separating effect can be effectively improved by changing the pressure in a counterbalance valve, changing the proportion of a modifying agent, changing the temperature of a chromatographic column and changing the flow rate of a mobile phase. The supercritical chromatographic analysis method has both the characteristics of gas phase chromatography and liquid phase chromatography; meanwhile, the supercritical chromatographic analysis method can not only be used for analyzing high-boiling-point low-volatility samples which are not adapted by the gas phase chromatography, but can also have quicker analytical speed and conditions than the efficient liquid chromatography, thus limitation of a method in the prior art is solved.

Description

technical field [0001] The invention specifically relates to a supercritical chromatographic analysis method for macamide components. Background technique [0002] Maca (Lepidium meyenii Walp.) is an annual herb of the family Brassicaceae (Lepidium L.), native to the Andes in Peru, South America. Because of its rich nutritional value and medicinal value, Maca has a long history of cultivation and consumption in the Andes. In 2011, the Ministry of Health of my country approved Maca as a new resource food. In the past 20 years, many studies have proved that Maca has the functions of improving the fertility of humans and animals, improving sexual function, inhibiting prostate enlargement, anti-fatigue, anti-depression, improving osteoporosis, and improving memory. Our country began to breed and plant in Lijiang, Yunnan in 2002, and achieved success. Since then, it has been planted in Tibet, Xinjiang, Qinghai and other places. Due to Maca's rich nutrition, diverse functions a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 潘云马晋芳葛发欢叶静
Owner SUN YAT SEN UNIV