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A method for identifying 10-hda in royal jelly preparation

A technology of 10-HDA and royal jelly, applied in the field of detection and analysis, can solve the problems of no relevant reports on the research of impurities, and achieve the effect of easy identification of authenticity, less operation steps, and sensitive response

Active Publication Date: 2021-05-14
XINYANG AGRI & FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are many related studies on 10-HDA, but they all focus on the detection of 10-HDA content in royal jelly preparations, but there are no relevant reports on the research on impurities in artificially synthesized 10-HDA

Method used

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  • A method for identifying 10-hda in royal jelly preparation
  • A method for identifying 10-hda in royal jelly preparation
  • A method for identifying 10-hda in royal jelly preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1 Comparison of 10-HDA extracted from royal jelly slag and artificially synthesized 10-HDA

[0043] Take 200 mg each of 10-HDA (97% content) extracted from royal jelly residue and 200 mg artificially synthesized 10-HDA (98% content), dissolve them in ethanol with a volume percentage of 95%, and set the volume to 100 mL. Use a 0.45 μm micropore After membrane filtration, RP-HPLC detection was carried out. Synthetic 10-HDA was purchased from Wuhan Yuancheng Gongchuang Technology Co., Ltd.

[0044] Equipment: Shimadzu LC-10AT high performance liquid chromatograph; Diamonsil C18 chromatographic column 5μm, 4.6×150mm.

[0045] Chromatographic conditions:

[0046] (1) The stationary phase is ODS-C 18 reversed phase column;

[0047] (2) The mobile phase is methanol: 0.03mol / L HCl: water (V / V / V)=55:10:35;

[0048] (3) The flow rate is 1.0mL / min;

[0049] (4) The detection wavelength is 210nm;

[0050](5) The injection volume is 10 μL.

[0051] see results figur...

Embodiment 2

[0052] RP-HPLC analysis of 10-HDA in the royal jelly preparation mixed with 0.5% artificially synthesized 10-HDA in embodiment 2

[0053] Synthetic 10-HDA was purchased from Wuhan Yuancheng Gongchuang Technology Co., Ltd.

[0054] Take 40 g of royal jelly preparation samples mixed with 0.5% artificially synthesized 10-HDA, dissolve them with 20 mL of 95% ethanol ultrasonically, and centrifuge to remove insoluble substances; put the filtrate on 30-60 mesh column chromatography silica gel, and use Elute with petroleum ether for 3 times the column volume, discard the eluate at this part; then elute with 50% ethanol with a volume percentage of 3 times the column volume to obtain the ethanol eluted part; recover the eluate until it has no ethanol smell , a white solid appears; continue to recover the aqueous phase to an appropriate volume, and filter with suction to obtain a white solid, which is blast-dried at 60°C for 6 hours and then set aside.

[0055] The above white solid wa...

Embodiment 3

[0064] RP-HPLC analysis of 10-HDA in the royal jelly preparation of embodiment 3 mixed with 1.0% artificially synthesized 10-HDA

[0065] Synthetic 10-HDA was purchased from Jiaxing Yuanmo Chemical Co., Ltd.

[0066] Take 50 g of royal jelly preparation samples mixed with 1.0% artificially synthesized 10-HDA, dissolve them with 20 mL of 95% ethanol ultrasonically, and centrifuge to remove insoluble adjuvants; the filtrate is loaded on 30 to 60 mesh column chromatography silica gel, and after the loading is completed, use 5 The petroleum ether of twice column volume was eluted, discarded the eluent of this part; Then eluted with 50% ethanol of the volume percentage of 4 times of column volume, obtained ethanol eluted part; A white solid appears; continue to recover the aqueous phase to an appropriate volume, and filter with suction to obtain a white solid, which is blown-dried at 60°C for 6 hours and set aside.

[0067] The above white solid was dissolved in 95% ethanol by vol...

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Abstract

The invention belongs to the technical field of detection and analysis, and specifically relates to an analysis and identification method for identifying whether artificially synthesized 10-HDA is mixed in a royal jelly preparation. The method adopts a silica gel column chromatography purification method to pre-treat the sample to be tested to obtain a white solid, and then It is detected by reverse-phase-high performance liquid chromatography, the stationary phase is ODS-C18 reverse-phase column, the volume ratio is 55:10:35 methanol:0.03mol / L HCl:water as the mobile phase, and isocratic elution is adopted. The identification method has high sensitivity, good separation and reproducibility, and obvious identification features, and can accurately identify the artificially synthesized 10-HDA mixed with more than 0.5% in the royal jelly preparation.

Description

technical field [0001] The invention belongs to the technical field of detection and analysis, and in particular relates to a method for identifying 10-HDA in royal jelly preparations. Background technique [0002] Royal jelly is the secretion from the head of worker bees. It is white or light yellow in color. It is an ideal natural health care product. It tastes sour, slightly sweet, and flat in nature; Soothing the liver and regulating qi, nourishing and strengthening, and improving immunity. The composition of royal jelly is extremely complex, and its main components include protein, various amino acids, vitamins, fatty acids, and biologically active enzymes. It has obvious health care effects on the human body, especially for cardiovascular diseases, blood lipid metabolism disorders, high blood pressure, endocrine disorders and other diseases. [0003] Royal jelly contains more than 26 kinds of fatty acids, 12 of which have been confirmed at present, among which 10-hyd...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027
Inventor 杨俊杰陈重郭磊磊潘岩郭心灵
Owner XINYANG AGRI & FORESTRY UNIV
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