CN104237230B - The quick determination method of epiphysin and its operation vessel combination - Google Patents
The quick determination method of epiphysin and its operation vessel combination Download PDFInfo
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- CN104237230B CN104237230B CN201410540275.4A CN201410540275A CN104237230B CN 104237230 B CN104237230 B CN 104237230B CN 201410540275 A CN201410540275 A CN 201410540275A CN 104237230 B CN104237230 B CN 104237230B
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Abstract
The present invention provides a kind of quick determination method of epiphysin and its operation vessel combination, this method comprise the following steps：Testing sample is dissolved with leaching liquor, is stood after concussion, to extract epiphysin；The supernatant liquor after dissolving is taken, the first developer and the second developer is successively added, observation solution change, precipitates if solution produces, be muddy, epiphysin is not contained in judgement sample；If not occurring precipitation, muddiness and not being changed into rose red color, epiphysin is not contained in judgement sample；If not occurring precipitation, muddiness and being changed into rose red color, contain epiphysin in judgement sample.The testing cost of the present invention is low, strong applicability, it is not necessary to which professional large-scale instrument is i.e. detectable, is adapted to general public to use, is particularly suitable for layman's quick detection melatonin in health products at the scene.
Description
Technical field
It is more particularly to a kind of to improve in sleep class health products whether add epiphysin the present invention relates to epiphysin detection method
Quick determination method and its operator vessel combination.
Background technology
Epiphysin（Melatonin, MT）It is a kind of indole hormone of generally existing in human body, mainly by pine in human body
Fruit glandular secretion, it has regulation circadian rhythm, sleep, endocrine and anti-ageing a variety of important physiological functions of waiting for a long time.
Because epiphysin has the good action of tranquilizing soporific, slept so there is part businessman to add a large amount of epiphysins in improvement
In the health products of dormancy class.But largely use can trigger breathing problem to epiphysin, disturb or cause whole internal system disorderly
Disorderly, so as to trigger other diseases.So there are strict requirements for the addition dosage of melatonin in health products.
The existing method for examining melatonin in health products content mainly has following four:
1st, thin-layered chromatography
Sample（Improvement sleep class health products to be detected）In composition to be measured extracted by methanol, the test sample of gained is molten
Liquid point is deployed on silica gel thin-layer plate with solvent, is taken out, is dried, put and inspected under uviol lamp 254nm.In the effect of solvent
Under, because the migration velocity of different material is different, different material occurs in the diverse location of chromatographic sheet in the form of spot,
Testing sample is judged according to the phenomenon obtained by whether testing sample spot this experiment occurs in position corresponding with reference substance
Whether target component is contained.If there is spot in need testing solution thin-layer chromatogram position corresponding with epiphysin reference substance,
It is there may be in prompting sample containing epiphysin composition
The advantages of thin-layered chromatography is analytical instrument that need not be expensive.Shortcoming is：（1）Chromatographic resolution rate is relatively low, Chinese medicine
Produce complicated component, disturbing factor is more, and some compositions that coexist easily are mistaken for into epiphysin composition, if it is some coexist composition amount compared with
Big and chromatographic mobile value approaches with composition to be measured, then can jamming target composition detection.（2）Development of chromatogram and the time dried
It is long, it is insufficient for the requirement quickly determined.（3）Chromatographic sheet needs to dry and dry storage, environment temperature and humidity
Separating effect is had a great influence.（4）Need fixed place, the big Site Detection of uncomfortable cooperation mobility.（5）It is realistic
The personnel of testing have preferable experience.
2nd, high performance liquid chromatography
High performance liquid chromatography is existing frequently-used analysis method, and under identical chromatographic condition, different materials has not
Same chromatographic retention.Epiphysin reference substance solution and need testing solution point obtained by sample extraction under identical chromatographic condition
Other sample introduction, it can determine whether testing sample contains epiphysin composition according to chromatographic peak retention time.
The advantages of high performance liquid chromatography is chromatographic isolation efficiency high, high sensitivity.Shortcoming is：（1）Instrument price is expensive,
Time for sample pretreatment is grown, and chromatographic column is vulnerable to pollution, and analysis cost is high；（2）When the chromatographic peak retention time coexisted is black with taking off
Plain color spectral peak retention time is apt to do false judgment when close；（3）Instrument requires use environment high, it is necessary to fixed placement, no
It is adapted to the big Site Detection of mobility
3rd, tablets by HPLC-MS
High performance liquid chromatograph is fitted as separator, mass spectrograph as the tablets by HPLC-MS of analyzer
Together in the serious sample analysis of complicated component, ambient interferences, this analysis method can improve the reliability of testing result.
4th, ELISA
Make antigen or antibody binding to certain solid phase surface, and keep its immunocompetence.Measure when, by inspection sample with
Either antibody reacts enzyme-labelled antigen according to the antigen or antibody of different step and surface of solid phase carriers.With the method for washing
Formation antigen antibody complex on solid phase carrier is set to be separated with other materials, the enzyme amount and sample being finally incorporated on solid phase carrier
The amount of middle examined object kind is proportional.After adding enzyme reaction substrate, substrate is changed into color products by enzymatic, the amount of product with
The amount of examined object in sample is directly related, it is possible to carries out qualitative or quantitative analysis according to the depth of color reaction.
To sum up, existing all kinds of methods can not all meet that the rapid detection of low cost, scene, the reality without professional are wanted
Ask.
The content of the invention
It is non-special to allow it is an object of the invention to provide a kind of quick determination method of epiphysin and its operation vessel combination
Industry personnel can detect in health products whether include epiphysin quickly, at low cost at the scene.
To achieve these goals, the present invention provides following technical scheme：
A kind of quick determination method of epiphysin, it comprises the following steps：Testing sample is dissolved with leaching liquor, it is quiet after concussion
Put, to extract epiphysin；The supernatant liquor after dissolving is taken, successively adds the first developer and the second developer, observation solution becomes
Change, if solution produces precipitation, muddiness, epiphysin is not contained in judgement sample；If do not occur precipitation, muddiness and be not changed into
Rose red color, then epiphysin is not contained in judgement sample；If not occurring precipitation, muddiness and being changed into rose red color, sentence
Contain epiphysin in disconnected sample.
In a kind of preferred embodiment of the quick determination method of above-mentioned epiphysin, the sample is slept for the improvement of solid-state
Class health products.
In a kind of preferred embodiment of the quick determination method of above-mentioned epiphysin, the leaching liquor is organic solvent.
In a kind of preferred embodiment of the quick determination method of above-mentioned epiphysin, the leaching liquor is ethanol.
In a kind of preferred embodiment of the quick determination method of above-mentioned epiphysin, first developer is that phosphomolybdic acid is molten
Liquid, second developer are vanillic aldehyde lysate.
In a kind of preferred embodiment of the quick determination method of above-mentioned epiphysin, first developer be concentration between
Phosphorus molybdenum acid solution between 2-8%, second developer are vanillic aldehyde solution of the concentration in 6-14g/L.
In a kind of preferred embodiment of the quick determination method of above-mentioned epiphysin, first developer is 3-7% phosphorus
Molybdenum acid solution；Second developer is 8-12 g/L vanillic aldehyde solution.
In a kind of preferred embodiment of the quick determination method of above-mentioned epiphysin, first developer is 4-6% phosphorus
Molybdenum acid solution；Second developer is 9-11 g/L vanillic aldehyde solution.
To achieve these goals, another technical scheme provided by the invention is as follows：
One kind operation vessel combination, it is used for the quick determination method of any of the above-described described epiphysin, including for holding
Receive the first container of leaching liquor, the second container for dissolving testing sample, the 3rd container for accommodating the first developer, use
In the 4th container for accommodating the second developer.
Analysis understands that testing cost of the invention is low, strong applicability, it is not necessary to which professional large-scale instrument is i.e. detectable, fits
Close general public to use, be particularly suitable for layman's quick detection melatonin in health products at the scene.
Embodiment
The present invention is described in further details with reference to embodiment.
In the epiphysin in using present invention detection health products, food, medicine, particularly it is used for the improvement for detecting solid-state
Sleep class health products in epiphysin when, following steps can be used：
From a container, such as a glassware, a little leaching liquor is taken out, is dissolved with leaching liquor in a container and treats test sample
Product, stood after concussion, to extract epiphysin.
The supernatant liquor after a little dissolving is taken out into a container, takes out a little first colour developing respectively from other two container
Agent, the second developer, and the first developer and the second developer are successively added in foregoing supernatant liquor, observation solution change,
If solution produces precipitation, muddiness, epiphysin is not contained in judgement sample；If do not occur precipitation, muddiness and be not changed into rose
Rare red color, then epiphysin is not contained in judgement sample；If not occurring precipitation, muddiness and being changed into rose red color, sentence
Contain epiphysin in disconnected sample.
Above-mentioned multiple containers and the liquid wherein accommodated can be concentrated and is accommodated in a kit, with convenient use, be carried.
Preferably, leaching liquor is organic solvent, it is highly preferred that the leaching liquor is ethanol.
Preferably, the first developer is phosphorus molybdenum acid solution, and the second developer is vanillic aldehyde lysate.For the dense of the two
Degree, the first chromogenic agent is between 2-8%, and the second chromogenic agent is between 6-14g/L.For example, the first developer is dense
Spend for 3%, 3.5%, 4-6%, 7%, the second chromogenic agent is 6%, 7%, 8-12 g/L, 12.5%, 14%；It is highly preferred that first is aobvious
Toner concentration is 4-6%, and the second chromogenic agent is 9-11 g/L.
It is highly preferred that how much the addition of two developers can regard supernatant liquor, 2-4 drops, such as 3 drops are selectively added
Deng.
In summary, the invention has the advantages that：Cost is low, and use condition is simple, it is not necessary to expensive analytical instrument,
Also without professional person, it is adapted to the common people to use.On-site rapid inspection epiphysin is suitable as, meets drugs and health care products supervision inspection
The needs tested.Also, the present invention has the characteristics that anti-impurity interference performance is strong, phenomenon is obvious, result is accurate.
As known by the technical knowledge, the present invention can pass through the embodiment party of other essence without departing from its spirit or essential feature
Case is realized.Therefore, embodiment disclosed above, for each side, all it is merely illustrative, is not only.Institute
Have within the scope of the present invention or be included in the invention in the change being equal in the scope of the present invention.
Claims (5)
1. a kind of quick determination method of epiphysin, it is characterised in that comprise the following steps：
Testing sample is dissolved with leaching liquor, is stood after concussion, to extract epiphysin；
The supernatant liquor after dissolving is taken, successively adds the first developer and the second developer, observation solution change, if solution produces
Precipitation, muddiness, then do not contain epiphysin in judgement sample；If not occurring precipitation, muddiness and not being changed into rose red color,
Epiphysin is not contained in judgement sample；If not occurring precipitation, muddiness and being changed into rose red color, contain in judgement sample and take off
Melanocyte；
First developer is phosphorus molybdenum acid solution, and second developer is vanillic aldehyde lysate；
The leaching liquor is the ethanol as organic solvent.
2. the quick determination method of epiphysin according to claim 1, it is characterised in that the sample is the improvement of solid-state
Sleep class health products.
3. the quick determination method of epiphysin according to claim 1, it is characterised in that first developer is concentration
Phosphorus molybdenum acid solution between 2-8%, second developer are vanillic aldehyde solution of the concentration in 6-14g/L.
4. the quick determination method of epiphysin according to claim 3, it is characterised in that first developer is 3-7%
Phosphorus molybdenum acid solution；Second developer is 8-12 g/L vanillic aldehyde solution.
5. the quick determination method of epiphysin according to claim 4, it is characterised in that first developer is 4-6%
Phosphorus molybdenum acid solution；Second developer is 9-11 g/L vanillic aldehyde solution.
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| CN105891364A (en) * | 2016-04-11 | 2016-08-24 | 北京洛奇临床检验所股份有限公司 | Method and kit for detecting melatonin in saliva with HPLC-MS/MS (high performance liquid chromatography-tandem mass spectrometry) technology |
| CN109239063A (en) * | 2018-09-29 | 2019-01-18 | 杭州天迈生物科技有限公司 | A kind of rapid detection method of melatonin in health products |
| CN114184441B (en) * | 2021-10-19 | 2024-04-05 | 威凯检测技术有限公司 | Preparation device and method of animal-derived medical instrument biosafety evaluation experiment leaching solution |
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| JP4172103B2 (en) * | 1999-07-14 | 2008-10-29 | 東ソー株式会社 | Method for measuring melatonin |
| CN100333651C (en) * | 2004-09-03 | 2007-08-29 | 光明乳业股份有限公司 | Method for purifying melatomin in milk product and detection method therefor |
| CN102393391B (en) * | 2011-10-18 | 2013-02-27 | 深圳市药品检验所 | Rapid measurement method of melatonin doped in Chinese patent medicine and healthcare food |
| CN103278499A (en) * | 2013-05-28 | 2013-09-04 | 无锡中德伯尔生物技术有限公司 | Method for testing melatonin |
| CN103969454B (en) * | 2013-12-18 | 2016-06-08 | 深圳市药品检验所 | Melatonin method for quick and detection thereof block and preparation method |
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