CN106706614B - Detect the kit and preparation method thereof of para hydroxybenzene alanine in urine - Google Patents
Detect the kit and preparation method thereof of para hydroxybenzene alanine in urine Download PDFInfo
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Abstract
Detect the kit of para hydroxybenzene alanine in urine, the ampoule bottle including being loaded with detection reagent, the ingredient of the detection reagent are as follows: nitric acid HNO3: 22~26%, sulfuric acid H2SO4: 20~24%, mercurous nitrate Hg2(NO3)2: 18~20%, mercuric sulfate HgSO4: 10~14%, nickel nitrate Ni (NO3)2: 7~8%, remaining is water；Another scheme is that the detection reagent is the chitosan composite fiber element aeroge for being adsorbed with tyrosinase and sodium metaperiodate.The present invention has the function of specific detection to para hydroxybenzene alanine micro in urine, and detection method is simple, quick, and accuracy rate is high.
Description
Technical field
The present invention relates to tumor markers detection technique fields, more particularly, to the third ammonia of para hydroxybenzene in a kind of detection urine
The kit and preparation method thereof of acid.
Background technique
Tumor markers refer in the generation and breeding of tumour, caused by tumour cell itself either by
What body generated tumour cell reaction, reflection tumour exists and a substance of growth, including protein, hormone, enzyme are (together
Work enzyme) and oncoprotein etc..The tumor markers in blood samples of patients or body fluid are chemically examined, early detection can be swollen in cancer screening
Tumor, and observe the curative effect of oncotherapy and judge patient's prognosis.
Para hydroxybenzene alanine (i.e. tyrosine) is used as tumor markers, is recognized by numerous scholars, such as
CN102004103, fast urine list hydroxyl phenol metabolism analyte detection in malignant tumour diagnostic value (laboratory medicine and clinical,
2016 the 6th phases, Li Xingcui etc.), urine para hydroxybenzene alanine detection in malignant tumour early prediction application value (examine
Medicine and clinical, the 16th phase in 2015, yellow-study plum etc.).
The advantages of these detection methods are inorganic chemical reagent detection method at present, inorganic chemistry detection method is detection reagent
Preparation is simple.But the content of the para hydroxybenzene alanine in urine is and its micro, and in urine there is also it is a variety of its
His Multiple components will affect testing result, therefore, develop it is a kind of it is more accurate, the higher detection method of specificity is extremely urgent.
Summary of the invention
In view of the above-mentioned problems existing in the prior art, the applicant provides para hydroxybenzene alanine in a kind of detection urine
Kit and preparation method thereof.The present invention has the function of specific detection to para hydroxybenzene alanine micro in urine, inspection
Survey method is simple, quick, and accuracy rate is high.
Technical scheme is as follows:
The kit of para hydroxybenzene alanine, the ampoule bottle including being loaded with detection reagent are described in a kind of detection urine
The ingredient of detection reagent are as follows:
Nitric acid HNO3: 22~26%, sulfuric acid H2SO4: 20~24%, mercurous nitrate Hg2(NO3)2: 18~20%, mercuric sulfate
HgSO4: 10~14%, nickel nitrate Ni (NO3)2: 7~8%, remaining is water.
Another scheme is that detection reagent can be the chitosan composite fiber element for being adsorbed with tyrosinase and sodium metaperiodate
Aeroge.The chitosan composite fiber element aeroge for being adsorbed with tyrosinase and sodium metaperiodate the preparation method comprises the following steps:
(1) native cellulose is dissolved, solvent is the solvent of conventional dissolution fiber, such as sodium hydroxide, urea, preparation
The concentration of obtained cellulose solution is controlled in 4wt%~6wt%, then cellulose solution is cast or is coated film-like, is passed through
Solidification regeneration and washing are prepared into the cellulose membrane with a thickness of 10~15 microns；
(2) one layer of chitosan solution is cast or coated on the cellulose membrane that step (1) is prepared, and dissolves chitosan
Solvent is Conventional solvents, such as acetic acid, and the chitosan concentration being prepared is in 3~5wt%；Obtained after solidification a layer thickness be 10~
15 microns of chitosan film；
(3) it is replaced with cellulose-chitosan complex film that dehydrated alcohol obtains step (2), removes water therein
Point, then cellulose-chitosan complex film reversion is placed, is located above cellulose membrane；
(4) one layer of chitosan is cast or coated on cellulose-chitosan complex film cellulose membrane that step (3) obtains
Solution obtains the chitosan film that a layer thickness is 10~15 microns, obtains chitosan-cellulose-chitosan complex film after solidification；
(5) chitosan-cellulose-chitosan complex film that step (4) obtains is replaced with dehydrated alcohol, removes it
In moisture, then freeze-dried or critical drying obtains chitosan-cellulose-chitosan composite aerogel；
(6) tyrosinase and sodium metaperiodate are uniformly mixed according to the ratio of 3~5:1 of mass ratio, are placed in deionized water and match
The suspension that mass fraction of solids is 10~12% is made, the composite aerogel that step (5) obtains then is put into the suspension
In, in water bath chader oscillation fix 3~5 hours to get.
The tyrosinase is commercially available mammal tyrosinase.Preferably, the tyrosinase is commercially available human tyrosine
Enzyme or rat tyrosinase.
It is nitric acid HNO for detection reagent3: 22~26%, sulfuric acid H2SO4: 20~24%, mercurous nitrate Hg2(NO3)2: 18
~20%, mercuric sulfate HgSO4: 10~14%, nickel nitrate Ni (NO3)2: 7~8%, remaining for for this detection method of water,
Detection method are as follows: be advisable for 20 DEG C of temperature or so when inspection, fresh clean voided (preferably urine) 3ml is taken to be added first time in the morning
In ampoule bottle equipped with reagent, shake up it is rear it is quiet put 3~5 minutes, then carry out colorimetric with colorimetric card, arrive yellow if it is colourless,
It is then negative；It is then weakly positive if it is lilac to pink colour；It is then positive if it is brown to dark-brown；If it is black
It is then in the presence of interference, can not judges.
For wherein detection reagent be adsorbed with tyrosinase and sodium metaperiodate chitosan composite fiber element aeroge this
For one detection method, detection method are as follows: be advisable for 20 DEG C of temperature or so when inspection, take fresh clean voided (preferably morning
First time urine) 3ml is added in the ampoule bottle equipped with reagent, shake up it is rear it is quiet put 3~5 minutes, then carry out colorimetric with colorimetric card,
Yellow is arrived if it is colourless, then is negative；It is then the positive if it is pink colour；It is then invalid if it is other colors.
Aeroge is a kind of porous material with nanostructure, and porosity is up to 90% or more, and density is minimum can be extremely
0.001g/cm3, it is most light one of solid material in the world at present.It differs markedly from hole configurations in micron and grade
Porous material, have great specific surface area.Due to its distinctive nanoporous, three-dimensional net structure, many is made it have
Unique performance.The microstructure of chitosan composite fiber element aeroge is that have the 3 D stereo of extra specific surface area network-like
Honeycomb is adsorbed with several tyrosinases in each small honeycomb.The knot for the double-deck aeroge that the present invention is prepared
Structure is more loose, and specific surface area is bigger, can achieve 500m2/ g, and cellulose and chitosan are all close biomaterials, no
Tyrosinase can be had an impact.
Tyrosinase is fixed in the hole of the double-deck aeroge by the method for immobilized enzyme, and this method can make tyrosine
Enzyme secure bond does not need cautious carrying in aeroge hole, is more suitable for ordinary people's purchase, transports and use.
And the distribution that the method for immobilised enzymes can make tyrosinase more uniform, and be monolayer distribution.This makes in aeroge
Gap in, with the presence of most single layer tyrosinases on per unit, when it encounters tyrosine, can there is highest
Sensitivity and reaction speed.
Tyrosinase is from commercially available human tyrosinase；Other mammals such as rat tyrosinase can also be used.Junket
It is rapidly catechol by tyrosine catabolic after propylhomoserin enzyme is contacted with the tyrosine in urine.Colour reagent is periodic acid
Sodium powder end, catechol react generation two a kind of jade of adjacent benzene with sodium metaperiodate, and pinkiness can be by being observed visually.
The present invention is beneficial to be had the technical effect that
Kit test method provided by the invention is simple, surveys certainly convenient for various crowds；Detection time is short, and color developing effect is bright
Aobvious, tester can judge without professional knowledge；Detection effect is sensitive, and accuracy rate is high, is suitable for a wide range of promote and apply.
Specific embodiment
Below with reference to embodiment, the present invention is specifically described.
Embodiment 1
The kit of para hydroxybenzene alanine, the ampoule bottle including being loaded with detection reagent are described in a kind of detection urine
The ingredient of detection reagent are as follows: nitric acid HNO3: 24%, sulfuric acid H2SO4: 22%, mercurous nitrate Hg2(NO3)2: 19%, mercuric sulfate
HgSO4: 12%, nickel nitrate Ni (NO3)2: 7.6%, remaining is water.
Its detection method are as follows: be advisable for 20 DEG C of temperature or so when inspection, taking fresh clean voided, (preferably urinate in the morning for the first time
Liquid) 3ml is added in the ampoule bottle equipped with reagent, shake up it is rear it is quiet put 3~5 minutes, then colorimetric is carried out with colorimetric card, if it is nothing
Color is then negative to yellow；It is then weakly positive if it is lilac to pink colour；It is then positive if it is brown to dark-brown；
It is then in the presence of interference if it is black, can not judges.
The Detection accuracy of this method is 93~95%.
Embodiment 2
The kit of para hydroxybenzene alanine, the ampoule bottle including being loaded with detection reagent are described in a kind of detection urine
Detection reagent is the chitosan composite fiber element aeroge for being adsorbed with tyrosinase and sodium metaperiodate.Preparation method are as follows:
(1) native cellulose is dissolved with sodium hydroxide, obtains the cellulose solution of 4wt%, then cellulose is molten
Film-like is prolonged or coated to liquid stream, by solidification regeneration and washing, is prepared into the cellulose membrane with a thickness of 10 microns；
(2) one layer of chitosan solution is cast or coated on the cellulose membrane that step (1) is prepared, and dissolves chitosan
Solvent is acetic acid, and the chitosan concentration being prepared is 5wt%；The chitosan film that a layer thickness is 10 microns is obtained after solidification；
(3) it is replaced with cellulose-chitosan complex film that dehydrated alcohol obtains step (2), removes water therein
Point, then cellulose-chitosan complex film reversion is placed, is located above cellulose membrane；
(4) one layer of chitosan is cast or coated on cellulose-chitosan complex film cellulose membrane that step (3) obtains
Solution obtains the chitosan film that a layer thickness is 10 microns, obtains chitosan-cellulose-chitosan complex film after solidification；
(5) chitosan-cellulose-chitosan complex film that step (4) obtains is replaced with dehydrated alcohol, removes it
In moisture, then freeze-dried or critical drying obtains chitosan-cellulose-chitosan composite aerogel；
(6) tyrosinase and sodium metaperiodate are uniformly mixed according to the ratio of mass ratio 3:1, are placed in deionized water and are configured to
The composite aerogel that step (5) obtains, is then put into the suspension, in water-bath by the suspension that mass fraction of solids is 12%
In oscillator oscillation fix 3 hours to get.The tyrosinase is commercially available human tyrosinase.
Its detection method are as follows: be advisable for 20 DEG C of temperature or so when inspection, taking fresh clean voided, (preferably urinate in the morning for the first time
Liquid) 3ml is added in the ampoule bottle equipped with reagent, shake up it is rear it is quiet put 3~5 minutes, then colorimetric is carried out with colorimetric card, if it is nothing
Color is then negative to yellow；It is then the positive if it is pink colour；It is then invalid if it is other colors.The detection of this method
Accuracy rate is 99% or more, and the recall rate of invalid state is below 0.001%.
Embodiment 3
The kit of para hydroxybenzene alanine, the ampoule bottle including being loaded with detection reagent are described in a kind of detection urine
Detection reagent is the chitosan composite fiber element aeroge for being adsorbed with tyrosinase and sodium metaperiodate.Preparation method are as follows:
(1) native cellulose is dissolved with sodium hydroxide and urea, obtains the cellulose solution of 6wt%, then will be fine
It ties up plain solution curtain coating or coating film-like and the cellulose membrane with a thickness of 15 microns is prepared by solidification regeneration and washing；
(2) one layer of chitosan solution is cast or coated on the cellulose membrane that step (1) is prepared, and dissolves chitosan
Solvent is acetic acid, and the chitosan concentration being prepared is 3wt%；The chitosan film that a layer thickness is 15 microns is obtained after solidification；
(3) it is replaced with cellulose-chitosan complex film that dehydrated alcohol obtains step (2), removes water therein
Point, then cellulose-chitosan complex film reversion is placed, is located above cellulose membrane；
(4) one layer of chitosan is cast or coated on cellulose-chitosan complex film cellulose membrane that step (3) obtains
Solution obtains the chitosan film that a layer thickness is 15 microns, obtains chitosan-cellulose-chitosan complex film after solidification；
(5) chitosan-cellulose-chitosan complex film that step (4) obtains is replaced with dehydrated alcohol, removes it
In moisture, then freeze-dried or critical drying obtains chitosan-cellulose-chitosan composite aerogel；
(6) tyrosinase and sodium metaperiodate are uniformly mixed according to the ratio of mass ratio 5:1, are placed in deionized water and are configured to
The composite aerogel that step (5) obtains, is then put into the suspension, in water-bath by the suspension that mass fraction of solids is 10%
In oscillator oscillation fix 5 hours to get.The tyrosinase is commercially available rat tyrosinase.
Its detection method are as follows: be advisable for 20 DEG C of temperature or so when inspection, taking fresh clean voided, (preferably urinate in the morning for the first time
Liquid) 3ml is added in the ampoule bottle equipped with reagent, shake up it is rear it is quiet put 3~5 minutes, then colorimetric is carried out with colorimetric card, if it is nothing
Color is then negative to yellow；It is then the positive if it is pink colour；It is then invalid if it is other colors.The detection of this method
Accuracy rate is 98.5% or more, and the recall rate of invalid state is below 0.003%.
Claims (3)
1. detecting the kit of para hydroxybenzene alanine in urine, the ampoule bottle including being loaded with detection reagent, which is characterized in that
The detection reagent is the chitosan composite fiber element aeroge for being adsorbed with tyrosinase and sodium metaperiodate；
The chitosan composite fiber element aeroge for being adsorbed with tyrosinase and sodium metaperiodate the preparation method comprises the following steps:
(1) native cellulose is dissolved, obtains cellulose solution, then cellulose solution is cast or is coated film-like, leads to
Supersolidification regeneration and washing, are prepared into the cellulose membrane with a thickness of 10~15 microns；
(2) one layer of chitosan solution is cast or coated on the cellulose membrane that step (1) is prepared, and a thickness is obtained after solidification
The chitosan film that degree is 10~15 microns；
(3) it is replaced with cellulose-chitosan complex film that dehydrated alcohol obtains step (2), removes moisture therein, so
Cellulose-chitosan complex film reversion is placed afterwards, is located above cellulose membrane；
(4) it is cast on cellulose-chitosan complex film cellulose membrane that step (3) obtains or one layer of chitosan of coating is molten
Liquid obtains the chitosan film that a layer thickness is 10~15 microns, obtains chitosan-cellulose-chitosan complex film after solidification；
(5) chitosan-cellulose-chitosan complex film that step (4) obtains is replaced with dehydrated alcohol, is removed therein
Moisture, then freeze-dried or critical drying, obtains chitosan-cellulose-chitosan composite aerogel；
(6) tyrosinase and sodium metaperiodate are uniformly mixed according to the ratio of 3~5:1 of mass ratio, are placed in deionized water and are configured to
The composite aerogel that step (5) obtains, is then put into the suspension by the suspension that mass fraction of solids is 10~12%,
In water bath chader oscillation fix 3~5 hours to get.
2. the kit of para hydroxybenzene alanine in detection urine according to claim 1, it is characterised in that the junket ammonia
Sour enzyme is commercially available mammal tyrosinase.
3. the kit of para hydroxybenzene alanine in detection urine according to claim 1, it is characterised in that the junket ammonia
Sour enzyme is commercially available human tyrosinase or rat tyrosinase.
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| CN201611021890.XA CN106706614B (en) | 2016-11-21 | 2016-11-21 | Detect the kit and preparation method thereof of para hydroxybenzene alanine in urine |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108152495A (en) * | 2017-12-27 | 2018-06-12 | 江苏华鸣生物科技有限公司 | A kind of colloid gold test paper for detecting tyrosine |
| CN108872221B (en) * | 2018-07-11 | 2020-05-22 | 深圳华创生物医药科技有限公司 | Lyophilized powder for detecting p-hydroxyphenylalanine and preparation method and application thereof |
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| HK1080146A1 (en) * | 2004-03-05 | 2006-04-21 | Egomedical Swiss Ag | Analyte test system for determining the concentration of an analyte in a physiological or aqueous fluid |
| CN101809165A (en) * | 2007-03-30 | 2010-08-18 | 高通量基因组学公司 | Measurement of an insoluble analyte in a sample |
| CN103323452A (en) * | 2013-06-21 | 2013-09-25 | 吉林生物研究院有限公司 | P-hydroxy phenylalanine urine detection reagent and preparation method thereof |
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