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Detection method of fatty acid compounds and/or sterol compounds in rape bee pollen

A technology for rape bee pollen and a detection method, which is applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve the problems of increasing analysis time, being unsuitable for detection, and complicating analysis methods, and achieves faster detection speed, improved detection sensitivity, precision The effect of increasing the degree of

Active Publication Date: 2013-05-08
JIANGSU KANION PHARMA CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the commonly used methods for the analysis and detection of fatty acid compounds and / or sterol compounds include gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS). , its disadvantages are side reactions such as oxidation, decomposition and isomerization during the esterification process, and it is difficult to ensure complete esterification, which increases the analysis time during the esterification process and complicates the analysis method, because both free fatty acids and fatty acid derivatives are Derived into fatty acid methyl esters, etc., these methods cannot be used to directly determine the content of non-derivatized fatty acid compounds and / or sterol compounds, and are not suitable for detection in the production process

Method used

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  • Detection method of fatty acid compounds and/or sterol compounds in rape bee pollen
  • Detection method of fatty acid compounds and/or sterol compounds in rape bee pollen
  • Detection method of fatty acid compounds and/or sterol compounds in rape bee pollen

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Embodiment 1: the pretreatment of rape bee pollen

[0051] Weigh 7 kg of pulverized rapeseed bee pollen (purchased from Anhui Xuancheng Baikang Bee Industry) and place it in a mixing bucket, add 28 L of distilled water, stir at room temperature for 4 hours, place it in a centrifuge and centrifuge at 5000 r / min for 20 minutes, pour The supernatant was removed to obtain 9 kg of extract, and the centrifugal precipitate was placed in a microwave dryer (Guiyang Xinqi Microwave Industry Co., Ltd.), the drying temperature was 60 ° C, and the drying was completed after 200 min. The power consumption was 97.7 kilowatts, and the drainage was 5.12 kg. The weight of the sample is 3.88kg, and the color of the sample has basically no change before and after drying.

[0052] The above-mentioned rapeseed bee pollen after microwave vacuum drying is crushed and passed through a 60-mesh sieve, and then put into a 10L extraction axe, the extraction kettle, the separation kettle I, and the ...

Embodiment 2

[0054] Embodiment 2: Detection of fatty acid compounds and / or sterol compounds in rapeseed bee pollen by HPLC-ELSD method

[0055] Instrument: waters 515 HPLC pump

[0056] ALLTECH ELSD 2000

[0057] Column: YMC J’sphere ODS-H80 (4.6mm×250mm, 4μm);

[0058] Mobile phase: acetonitrile-water gradient elution (0min: 40:60, 10min: 60:40, 20min: 80:20, 30min: 100:0, 35min: 100:0);

[0059] Mobile phase flow rate: 1.00ml / min;

[0060] Column oven temperature: 35°C;

[0061] ELSD drift tube temperature: 85°C;

[0062] ELSD gas: air;

[0063] ELSD gas flow rate: 3.0L / min;

[0064] 1. Linear relationship experiment:

[0065] Preparation of reference solution: Accurately weigh 14.47mg of linolenic acid amide reference substance, 8.26mg of linolenic acid glyceride reference substance, 39.85mg of linolenic acid reference substance, and 20.92mg of palmitic acid reference substance in a 25ml volumetric flask, dissolve with methanol and determine To obtain a mixed standard solution o...

Embodiment 3

[0081] Example 3: Detection of fatty acid compounds and / or sterol compounds in rapeseed pollen by HPLC-UV method

[0082] Instrument: Agilent 1260HPLC

[0083] Chromatographic column: YMC J’sphere ODS-H80 (4.6mm×250mm, 4μm);

[0084] Mobile phase: acetonitrile-acid water gradient elution (0min: 70:30, 10min: 80:20, 20min: 90:10, 40min: 90:10, acid is aqueous solution of phosphoric acid, formic acid, acetic acid, pH is 2)

[0085] Flow rate; 1ml / min;

[0086] Column oven; 35°C;

[0087] Detection wavelength; 205nm

[0088] 1. Linear relationship experiment

[0089] Preparation of reference substance solution: Accurately weigh 20.74 mg of 10-methoxy-1-heptadecene-4,6-diynyl-3,9-diol reference substance, 9.10 mg of oleic acid reference substance, Decanedioic acid reference substance 18.65mg, 12-methyl-myristate methyl ester reference substance 8.75mg, linolenic acid reference substance 76.15mg, oleic acid reference substance 16.82mg, anacardic acid A reference substance 21.3...

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Abstract

Disclosed is a detection method of fatty acid compounds and / or sterol compounds in rape bee pollen, which is characterized by comprising: a) pretreating the rape bee pollen to-be-measured to get rape bee pollen extracts; and b) detecting fatty acids and / or sterol compounds in rape bee pollen extracts by HPLC-ELSD and HPLC-UV method. The detection method of fatty acid compounds and / or sterol compounds in rape bee pollen is high in controllability and low in energy consumption, and is conductive to industrial production.

Description

technical field [0001] The invention belongs to the field of traditional Chinese medicine pharmacy, and in particular relates to a method for detecting fatty acid compounds and / or sterol compounds in rape bee pollen. Background technique [0002] Clinical practice at home and abroad has proved that pollen and its preparations are ideal drugs for the treatment of prostate diseases. Li Yonghui (Li Yonghui. Research on the pharmacodynamic substance basis of vegetable pollen against benign prostatic hyperplasia. Master's degree thesis of Shanghai Institute of Pharmaceutical Industry (D), 2009) reported in the literature that rape bee pollen, vegetable pollen, corn pollen, For pine pollen and sunflower pollen, more than 10 kinds of pollen of different varieties and different production areas were collected in major production areas of the country. Anti-inflammatory and anti-testosterone propionate-induced hyperplasia in rats were used as pharmacological screening models. Aspirin,...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/89
Inventor 杨义芳韦洁杨必成
Owner JIANGSU KANION PHARMA CO LTD
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