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Extraction and detection method for hormone substances in Antarctic krill

An Antarctic krill and extraction liquid technology, which is applied in the field of ultra-high performance liquid chromatography-mass spectrometry combined detection, can solve the problems of complex radioimmunization operation, high method false positives, and high detection limit, and achieves less impurities, simple operation, and high detection efficiency. low limit effect

Inactive Publication Date: 2018-11-30
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The operation of radioimmunoassay is complicated, and the equipment required is expensive. These synthetic substances are non-volatile and need to undergo silane methylation or acetylation reactions to convert them into volatile components before they can be determined by GC-MS. The sensitivity of ELISA is high. However, the method has high false positives and can only be used for qualitative primary screening
Thin-layer chromatography is a semi-quantitative detection method, which is fast and easy to operate, but has a high detection limit and requires more materials

Method used

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  • Extraction and detection method for hormone substances in Antarctic krill
  • Extraction and detection method for hormone substances in Antarctic krill
  • Extraction and detection method for hormone substances in Antarctic krill

Examples

Experimental program
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Effect test

Embodiment 1

[0076] Optimization of Chromatography and Mass Spectrometry Conditions

[0077] The selection of the mobile phase of ultra-high performance liquid chromatography conditions in the present disclosure has investigated methanol, water; methyl alcohol, acetonitrile; As the mobile phase, it was found that almost all hormones peaked within 3 minutes, and they were difficult to separate. Afterwards, methanol and 0.1% formic acid water were used as the mobile phase, and it was found that a gradient separation effect was not good. After continuously adjusting the mobile phase, it was found that methanol The effect of gradient separation with 0.1% formic acid water is better, and the peak can be completely separated within 9 minutes, and finally determined as the detection mobile phase.

[0078] The choice of flow rate, considering that the greater the flow rate, the lower the efficiency of ionization, the general flow rate will be selected between 0.1mL / min-0.3mL / min, the sensitivity i...

Embodiment 2

[0085] There are many kinds of steroid hormones contained in Antarctic krill, including estriol, cortisone, testosterone propionate, megestrol acetate, progesterone caproate, cortisone acetate, dexamethasone, nandrolone, prednisolone Nisolone, aldosterone, testosterone, estradiol, progesterone, hydrocortisone, diethylstilbestrol, norethindrone, etc., all belong to fat-soluble substances, which have caused great difficulties to effectively extract them, but the inventor It is found that some of the properties of these substances are quite different, and the chemical structures of some substances are very similar. The inventors use different organic solvents, hydrolysis methods and purification column combinations to extract them respectively according to their specific chemical structures and polarity differences. A very good extraction effect can be achieved.

[0086] This disclosure investigates and adopts ethyl acetate, methanol, acetonitrile respectively as extraction solve...

Embodiment 3

[0104] Take 10g of fresh Antarctic krill and freeze-dry it at -40°C. Freeze-dried Antarctic krill were ground and pulverized with a high-speed tissue grinder. Add 10 mL of ethyl acetate, vortex extract for 2 min, take the supernatant, repeat the extraction once, combine the supernatant, add 5 mL of sodium hydroxide buffer solution with pH=12, vortex extract for 1 min, centrifuge at 4000 r / min for 5 min, and take The supernatant was extracted with a QuEChERS solid-phase extraction cartridge, vortexed for 2 min, and centrifuged at 4000 r / min for 5 min. The supernatant was taken, evaporated to dryness, reconstituted with 1 mL of ethyl acetate, and passed through a 0.2 μm filter membrane. Obtain the crude extract from Antarctic krill. Bold materials were detected by ultra-high performance liquid chromatography established in Example 1. The contents of cortisone, testosterone propionate, megestrol acetate, progesterone caproate, cortisone acetate, dexamethasone and nandrolone in ...

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Abstract

The invention relates to an extraction and detection method for hormone substances in Antarctic krill. The method comprises the steps of refrigerating and drying the Antarctic krill, grinding and crushing Antarctic krill after refrigerating and drying; extracting the crushed and ground Antarctic krill by using ethyl acetate, thus acquiring first extracting solution; extracting the first extractingsolution by using sodium hydroxide buffer solution, thus acquiring second extraction solution; edulcorating and purifying the second extraction solution by using a QuEChERs solid phase extraction column, separating after purification, and taking supernate; and dehydrating the supernate, then redissolving by using the ethyl acetate, filtering by a membrane, thus acquiring extractives including cortisone, testosterone propionate, megestrol acetate, hydroxyprogesterone caproate, cortisone acetate, hexadecadrol and nandrolone. The extraction method provided by the invention is simple in operationprocess, short in consumed time, and capable of fully removing purities.

Description

technical field [0001] The disclosure belongs to the technical fields of medicine, food and chemical industry, in particular to a preparation of cortisone, testosterone propionate, megestrol acetate, progesterone caproate, cortisone acetate, dexamethasone and nandrolone in Antarctic krill High-efficiency extraction method and ultra-high performance liquid chromatography-mass spectrometry detection method. Background technique [0002] The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art. [0003] Cortisone, molecular formula: C 21 h 28 o 5 , Molecular weight: 360.44, cortisone is an adrenocortical hormone drug, mainly used in the replacement therapy of adrenal insufficiency and pituitary insufficiency, and can also be used for allergic and inflammatory diseases. Testosterone Propionate, molecular formula: C 22 h 32 o 3 , molecular weight: 344.49, testosterone propionate is an androge...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 韩香凝刘代成
Owner SHANDONG NORMAL UNIV
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