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Method for discriminating true and false of propolis through combination of fingerprint spectrum and antioxidation activity

A technology of antioxidant activity and fingerprint spectrum, applied in the field of quality identification of propolis raw materials, can solve problems such as component differences

Active Publication Date: 2018-06-15
SHANGHAI JIAODA ONLLY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But as mentioned above, even if the same propolis is produced by poplar gum vegetation in China, the composition of plant sources in different regions is very different

Method used

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  • Method for discriminating true and false of propolis through combination of fingerprint spectrum and antioxidation activity
  • Method for discriminating true and false of propolis through combination of fingerprint spectrum and antioxidation activity
  • Method for discriminating true and false of propolis through combination of fingerprint spectrum and antioxidation activity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0118] 1. Fingerprint Determination Steps

[0119] 1 Sample pretreatment

[0120] Get the sample of Example 1, freeze overnight, crush the next day, accurately weigh 1315.2g, place in a 25ml volumetric flask, add 95% ethanol to the mark, ultrasonically extract for 30min at normal temperature, use 95% ethanol to constant volume, centrifuge (5000rpm , 15 minutes), draw 0.5ml, to 10ml volumetric flask, with 95% ethanol constant volume, make propolis test sample ethanol solution 2.63mg / ml, cross 0.45um filter membrane in the sample bottle, wait for HPLC analysis.

[0121] 3.2 Fingerprint Determination Determination

[0122] 3.2.1 Chromatographic conditions

[0123] Chromatographic column: Venusil MP C18 250mm×4.6mm×5μm;

[0124] Mobile phase: methanol+0.4% phosphoric acid (V / V)=65+35;

[0125] Column temperature: 25°C; injection volume: 10μl; flow rate: 1ml / min; detection wavelength: 360nm.

[0126] 3.2.2 Determination

[0127] Inject 10 μl of sample liquid into the high per...

Embodiment 2

[0161] 1. Fingerprint Determination Steps

[0162] 1 Sample pretreatment

[0163]Get the sample of Example 2, freeze overnight, crush the next day, accurately weigh 705.2mg, place in a 25ml volumetric flask, add 95% ethanol to the mark, ultrasonically extract for 30min at normal temperature, dilute to volume with 95% ethanol, centrifuge (5000rpm , 15 minutes), draw 0.5ml to a 10ml volumetric flask, and use 95% ethanol to constant volume to prepare propolis test sample ethanol solution 1.41mg / ml, pass through a 0.45um filter membrane in the sample bottle, and wait for HPLC analysis.

[0164] 3.2 Fingerprint Determination Determination

[0165] 3.2.1 Chromatographic conditions

[0166] Chromatographic column: Venusil MP C18 250mm×4.6mm×5μm;

[0167] Mobile phase: methanol+0.4% phosphoric acid (V / V)=65+35;

[0168] Column temperature: 28°C; injection volume: 10 μl; flow rate: 1.2ml / min; detection wavelength: 360nm.

[0169] 3.2.2 Determination

[0170] Inject 10 μl of sampl...

Embodiment 3

[0206] 1. Fingerprint Determination Steps

[0207] 1 Sample pretreatment

[0208] Get the sample of Example 1, freeze overnight, crush the next day, accurately weigh 606.1g, place in a 25ml volumetric flask, add 95% ethanol to the mark, ultrasonically extract for 30min at normal temperature, dilute to volume with 95% ethanol, centrifuge (5000rpm , 15 minutes), draw 0.5ml, to 25ml volumetric flask, with 95% ethanol constant volume, make propolis test sample ethanol solution 0.48mg / ml, cross 0.45um filter membrane in the sample bottle, wait for HPLC analysis.

[0209] 3.2 Fingerprint Determination Determination

[0210] 3.2.1 Chromatographic conditions

[0211] Chromatographic column: Venusil MP C18 250mm×4.6mm×5μm;

[0212] Mobile phase: methanol+0.4% phosphoric acid (V / V)=65+35;

[0213] Column temperature: 25°C; injection volume: 10 μl; flow rate: 0.7ml / min; detection wavelength: 360nm.

[0214] 3.2.2 Determination

[0215] Inject 10 μl of sample liquid into the high pe...

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Abstract

The invention discloses a method for discriminating true and false of propolis through combination of fingerprint spectrum and antioxidation activity, which belongs to the quality discriminating of traditional Chinese medicine raw material quality control category, and specially relates to the method for identifying the true and false of the propolis raw material and its product by the high-pressure liquid-phase fingerprint spectrum and special antioxidation characteristic of the propolis. The method comprises three steps of fingerprint spectrum determination, oxyradical absorption capabilitydetermination and sample identification. Under same test condition, the fingerprint spectrum of a sample is compared with the fingerprint spectrum for simultaneously detecting the propolis and a poplar gum sample, several characteristic peaks in the fingerprint spectrum of the sample are selected, and true, false or adulteration of the propolis can be determined by convenient comparison and resultdetermination. The antioxidation specific index limitation and the fingerprint spectrum are combined for identifying the true, false or adulteration of the propolis.

Description

technical field [0001] The invention belongs to the quality identification of propolis raw materials in the quality control category of traditional Chinese medicine raw materials, and particularly relates to a method for jointly identifying the authenticity of propolis raw materials and products thereof by using high-pressure liquid phase fingerprints and the unique anti-oxidation properties of propolis. Background technique [0002] Modern studies have proved that the rich and unique active ingredients contained in propolis make it antibacterial, anti-inflammatory, antipruritic, anti-oxidant, immune-enhancing, blood sugar-lowering, blood-fat-lowering and other functions. Propolis is known as natural immune stimulant, natural antioxidant and natural antibacterial. Due to its broad and significant physiological activities and relatively low toxicity, the market size is constantly expanding. And because propolis is the resin (gum) collected by bees from plant buds or trunks, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N21/64
CPCG01N21/643G01N30/02
Inventor 邵卫樑杭晓敏夏祎稚施云
Owner SHANGHAI JIAODA ONLLY CO LTD
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