CN107621499A - 25 hydroxy vitamin D2s and 25 hydroxycholecalciferol high performance liquid chromatography MS detection kits - Google Patents
25 hydroxy vitamin D2s and 25 hydroxycholecalciferol high performance liquid chromatography MS detection kits Download PDFInfo
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- CN107621499A CN107621499A CN201610554486.2A CN201610554486A CN107621499A CN 107621499 A CN107621499 A CN 107621499A CN 201610554486 A CN201610554486 A CN 201610554486A CN 107621499 A CN107621499 A CN 107621499A
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Abstract
The present invention provides a kind of 25 hydroxy vitamin D2s and 25 hydroxycholecalciferol high performance liquid chromatography MS detection kits, including quality-control product, Isotopic Internal Standard extract solution, dilution, conversion fluid, redissolution liquid, Mobile Phase Additives A, Mobile Phase Additives B.This kit can detect 25 hydroxy vitamin D2s and 25 hydroxycholecalciferols respectively, and the used time is shorter, and detection efficiency is high, and detection sensitivity is high.
Description
Technical field
It is efficient more particularly to 25-OH Vintamin D2 and 25-hydroxyvitamin D3 the present invention relates to Mass Spectrometer Method field
Liquid chromatography mass is combined method detection kit
Background technology
Vitamin D is sterol analog derivative, ergosterol, vitamin D2, has anti-rachitic effect, also known as anti-rickets
Sick vitamin vitamin D family member includes vitamine D1, D2, D3, D4 and D5, and closer to healthy relation is D2 (ergots
Calciferol) and D3 (courage solidification alcohol) it be merely not only a kind of liposoluble vitamin, be substantially the one of a variety of physiologically actives of tool
Kind hormone, there is extensive physiological metabolism activated vitamin D, which to lack, can cause the diseases such as rickets, tetany, osteomalacia, but
It is to take in excessive vitamin D for a long time, the level of vitamin D in blood vessel and organ calcification therefore periodic detection human body will be caused,
For weighing body vitamin D supplementary results, and health is maintained to have great importance
Vitamin D can be synthesized by skin or food intake produce vitamin D half-life period about 3 hours, and with dimension
Raw plain D associated proteins are together；About 24 hours 1,25- (OH) 2 calciferols/D3 half-life period, content is extremely low in blood；25- hydroxyls
Base vitamin D is the mark being detected in blood, relatively stable because its half-life period is about 3 weeks, is vitamin D in human body again
Major storage form, by detection it may determine that the situation vitamin D of overall vitamin D be maintain bone health it is main
The famine of vitamin D will cause skeleton deformity element childhood, i.e. rickets vitamin D deficiency is Secondary cases parathyroid gland
The common disease factor 25-hydroxy-vitamin D content of Hyperactivity it is low also with bone density it is low it is relevant combined with other clinical datas, examine
Surveying result helps to judge that Bone m etabolism discovered in recent years vitamin D and cancer, angiocardiopathy, diabetes etc. have correlation,
Vitamin D level has certain prevention effect to cancer, multiple sclerosis, diabetes etc. inside enough
The crowd of vitamin D deficiency can improve internal vitamin D content by food, sunlight and vitamin replenisher,
Food source includes yolk, salmon, tuna, cod-liver oil, beef liver, margarine, Yoghourt, cheese etc.；What replenishers provided
Vitamin D includes two kinds of forms：D2 and two kinds of forms of D3 are all effective, each can ensure abundance vitamin D level but
It 2 and 3 is that incoordinate D3 is form caused by human body to be, there are some researches show D3 quickly improve can on vitamin D level recently
Up to 3 times, and it is 70 years old old that more permanent replenishers amount can be maintained, which to depend on the dietary standard that age and hazards are recommended,
Artificial 600IU/ days, 71 and for 800IU/ days, some researchers proposed above, vitamin D content height can bring a variety of health benefits
Place, but can damage too much according to United States Medicine research institute, more than 4000IU/ days, the risk of harm can increase
25 (OH) D2 and 25 (OH) D3 activity and therapeutic effect difference are big, and vitamine D3 should be used as preferred replenishers, but tie up
Raw plain D2 is also indispensable, and separate detection is that independent evaluation calciferol and vitamine D3 activity and function are inevitable requirements；Only
Detection 25-hydroxyvitamin D3 can cause total 25-hydroxy-vitamin D horizontal inaccurate, detect 25- hydroxyls D2/D3 ability respectively
Correct the effect of assessing vitamin D level and vitamin D replacement therapy, therefore determining 25-OH Vintamin D2/D3 respectively can be with
Directly reflect the level of vitamin D Actual activity in organism, there is important clinical meaning and efficacy determination meaning
However, although the detection method for having some to be directed to 25 (OH) D2 and 25 (OH) D3 in the prior art, is often grasped
It is relatively low to make complex (if desired for extraction step), detection sensitivity, and is difficult to simultaneous quantitative detection 25 (OH) D2 and 25
(OH)D3
Therefore, this area there is an urgent need to develop new detection sensitivity it is higher and can simultaneous quantitative detect 25 (OH) D2
With 25 (OH) D3 technology
The content of the invention
It is higher it is an object of the invention to provide a kind of detection sensitivity and can simultaneous quantitative detect 25 (OH) D2 and
25 (OH) D3 technology
In the first aspect of the present invention, there is provided a kind of high performance liquid chromatography MS detection kit, including：
(1) quality-control product, 25-OH Vintamin D2 and 25-hydroxyvitamin D3 are contained in described quality-control product；
(2) Isotopic Internal Standard extract solution, in described Isotopic Internal Standard extract solution containing 25-OH Vintamin D2-d3 and
25-hydroxyvitamin D3-d3；
(3) dilution, described dilution are acetonitrile；
(4) conversion fluid, described conversion fluid are PTAD (4- phenyl -1,2,4- triazolines -3,5- diketone)；
(5) liquid is redissolved, described redissolution liquid is methanol；
(6) Mobile Phase Additives A, described Mobile Phase Additives A are saturated monocarboxylic acid；
(7) Mobile Phase Additives B, wherein described Mobile Phase Additives B is C1-C3 amines
In another preference, described C1-C3 amines is selected from the group：Methylamine, ethamine, propylamine or its combination
In another preference, the kit also includes the part being selected from the group：
96 hole reaction plates, specification
In another preference, described kit also includes the part being selected from the group：
Reference substance is used to establish standard curve
In another preference, described Mobile Phase Additives B is methylamine
In another preference, the saturated monocarboxylic acid is formic acid, acetic acid, propionic acid, butyric acid or its combination
In another preference, the saturated monocarboxylic acid is formic acid
In another preference, the saturated monocarboxylic acid is one or a combination set of methanol and ethanol
In another preference, the saturated monocarboxylic acid is methanol
In the second aspect of the present invention, there is provided determined by tandem mass spectrometry one or more in taken biological sample
The method of the amount of dihydroxyvitamin D metabolites, including：
(i) one or more hydroxy vitamin D metabolites and internal standard are entered by using electric spray ion source (ESI)
Row ionization, produces one or more hydroxy vitamin D metabolites and the interior target at least one precursor ion respectively；
(ii) precursor ion described in one or more hydroxy vitamin D metabolites and the interior target is produced respectively
One or more fragment ions；With
(iii) in comparison step (i) or (ii) or both caused one or more hydroxy vitamin D metabolites and
The amount of the one or more ions of interior target is given birth to the one or more hydroxyl dimensions determined in the biological sample
The amount of plain D metabolins；
Wherein, methylamine is added in the mobile phase in chromatogram detection process
In another preference, wherein one or more dihydroxyvitamin D metabolites include 25- hydroxy vitamins
D2；And the matter of the parent ion of wherein described 25-OH Vintamin D2/lotus ratio is 619.3 ± 0.5
In another preference, wherein one or more dihydroxyvitamin D metabolites include
25-hydroxyvitamin D3；And the matter of the parent ion of wherein described 25-hydroxyvitamin D3/lotus ratio is
607.3±0.5
In another preference, wherein it is 298.3 ± 0.5 that one or more fragment ions, which are included selected from matter/lotus ratio,
Ion one or more ions
It should be understood that within the scope of the present invention, above-mentioned each technical characteristic of the invention and have in below (eg embodiment)
It can be combined with each other between each technical characteristic of body description, so as to form new or preferable technical scheme as space is limited,
This no longer tires out one by one states
Brief description of the drawings
Fig. 1 is 25-OH Vintamin D2 standard items chromatogram
Fig. 2 is 25-OH Vintamin D2-d3 Isotopic Internal Standard chromatograms
Fig. 3 is 25-hydroxyvitamin D3 standard items chromatogram
Fig. 4 is 25-hydroxyvitamin D3-d3 Isotopic Internal Standard chromatograms
Fig. 5 is 25-OH Vintamin D2 canonical plotting
Fig. 6 is 25-hydroxyvitamin D3 canonical plotting
Embodiment
The present inventor, by largely screening, develops a kind of high performance liquid chromatography first by in-depth study extensively
MS, methods described use specific mobile phase and specific Mass Spectrometer Method condition, not only simplify operation, and can
With in one-time detection simultaneous quantitative detect 25-OH Vintamin D2 and 25-hydroxyvitamin D3, and testing result is sensitive
Degree is high, and testing result accuracy height completes the present invention on this basis
Term
As used herein, term " 25-OH Vintamin D2-d3 " and " 25-OH Vintamin D2-2H " is used interchangeably,
Point out H is formed after being substituted by isotope deuterium in 25-OH Vintamin D2 deuterated thing in the present invention, it is used as 25-
The internal standard of hydroxy vitamin D2 Mass Spectrometer Method
As used herein, term " 25-hydroxyvitamin D3-d3 " and " 25-hydroxyvitamin D3-2H " is used interchangeably,
Point out H is formed after being substituted by isotope deuterium in 25-hydroxyvitamin D3 deuterated thing in the present invention, it is used as 25-
The internal standard of hydroxycholecalciferol Mass Spectrometer Method
Detection method
As used herein, " liquid chromatography " (LC) refers to when fluid is equably by the post or logical of trickle separated material
The method delay of one or more compositional selectings delay of fluid solution is due to when the fluid phase when crossing capillary channel filtering
The component of mixture is in one or more stationary phases and bulk fluid (bulk fluid) during for stationary phase (or multiple) movement
It is rapid that distribution " liquid chromatography " between (i.e. mobile phase) includes Reversed-phase liquid chromatography (RPLC), high performance liquid chroma- tography (HPLC) and height
Flow liquid chromatography (HTLC)
As used herein, term " HPLC " or " high performance liquid chroma- tography " refer to such liquid chromatography, wherein separation degree
It is by making mobile phase under pressure through stationary phase be usually tightly packed post and increased
As used herein, " mass spectrography " (MS) refers to the analytical technology MS technologies one by their Quality Identification compound
As include (1) compound is ionized to form charging cpd；(2) detect the molecular weight of charging cpd and calculate mass-to-charge ratio
(m/z) compound, which can by any suitable means ionize and detect " mass spectrograph ", generally comprises electro-dissociator and ion detector
Term " electron ionization " refers to such method, the wherein analysis interested in gaseous state or steam phase as used herein
Thing and the interaction of electron stream interaction electronics and analyte produce analyte ions, then it can be used for mass spectrometry art
Term " chemi-ionization " refers to such method as used herein, and wherein reagent gas (such as ammonia) touches for electronics
Hit, and analyte ions are interacted by reagent gas ion and analyte molecule to be formed
Term " ionization " refers to the analysis for producing the net charge with equal to one or more electron units as used herein
The process anion of thing ion is the ion of the net negative charge with one or more electron units, and cation is that have one
Or the ion of the net positive charge of multiple electron units
Term " about " refers to institute's indicating value plus or minus 10% when referring to quantitative measurment as used herein
Kit
Refer to the quality-control product containing the present invention, Isotopic Internal Standard extract solution, dilution, conversion present invention also offers a kind of
Liquid, liquid, Mobile Phase Additives A, Mobile Phase Additives B kit are redissolved, in the preference of the present invention, described examination
Agent box also includes the kits such as container, operation instructions, reference substance and can be used for detecting 25-OH Vintamin D2 in sample simultaneously
With 25-hydroxyvitamin D3 content
Typically, detection method includes following：
First, internal standard extract solution prepares：
The amount of Isotopic Internal Standard extraction working solution is calculated according to this test specimen amount, by 1:100 put forward the internal standard of concentration
Take liquid to be diluted with dilution, pay attention to fully mixing
Extraction:
Take 100 μ L human serums to add 500 μ L internal standard extract solutions, centrifuged after fully mixing, then pipette supernatant to 96 holes
In reaction plate, nitrogen drying
It is derivative：
100 μ L conversion fluid is added into 96 hole reaction plates of drying, after fully mixing, room temperature derives 1 hour
Redissolve：
Add 50 μ L and redissolve liquid, fully mix
2nd, liquid-phase condition
Mobile phase prepares
A phases：By 1:Mobile Phase Additives A is added in the aqueous solution by 1000 ratio
B phases：By 1:Mobile Phase Additives A, Mobile Phase Additives B are added in methanol by 1000 ratio respectively
Liquid chromatogram is eluted using gradient mode, and liquid phase chromatogram condition includes：
Chromatographic column：Octadecylsilane chemically bonded silica is filler or suitable person
Chromatographic column column temperature：40℃
Sample size：5μL
Flow velocity：0.5mL/min
Gradient：0-0.6min：Mobile phase B is 70%-100%；0.6-1.2min：Mobile phase B is 100%；1.2-
1.21min：Mobile phase B is 100%-70%；1.21-3.0min：Mobile phase B is 70%
Run time：3min
3rd, Mass Spectrometry Conditions
Multiple-reaction monitoring ion pair (MRM) and corresponding voltage parameter
Other mass spectrometry parameters
Ion gun：Electron spray (ESI) ion gun
Ionizing voltage：5500V
Auxiliary plus hot air temperature：550℃
Atomization gas (GAS1)：60psi
Auxiliary heating gas (GAS2)：60psi
Gas curtain gas (CUR)：20psi
Collision gas (CAD)：4psi
4th, upper machine testing
The reference substance handled well, quality-control product and test sample solution injection high performance liquid chromatography-tandem mass instrument is taken to carry out
Detection, and record in peak area and isotope of the chromatogram with detecting sample 25-OH Vintamin D2,25-hydroxyvitamin D3
Mark 25-OH Vintamin D2-d3,25-hydroxyvitamin D3-d3 peak areas
5th, quantitative analysis
The method for drafting of standard curve：Using the sign concentration of 7 reference substances as abscissa (x), with the reality of 7 reference substances
The ratio for detecting peak area and respective internal standard peak area is ordinate (y), draws standard curve
The fitting of calibration curve equation：Sign concentration (x) is linearly returned with the peak area ratio (y) of 7 reference substances
Regression equation can be obtained by returning：Y=a+bx, wherein y are ordinate, and x is abscissa, and a is intercept, and b is slope
Detect the calculating of sample results：The ratio of the actual peak area and internal standard peak area that detect sample is substituted into above-mentioned mark
Directrix curve equation, calculate the concentration of testing compound in detection sample
Main advantages of the present invention include：
(a) this kit can detect 25-OH Vintamin D2 and 25-hydroxyvitamin D3 respectively, be not required to extract in operation
Take, therefore process is easy, the used time is short, and the matter of the parent ion of 25-OH Vintamin D2/lotus ratio is tieed up for 619.3 ± 0.5,25- hydroxyls
Matter/lotus ratio of raw plain D3 parent ion is 607.3 ± 0.5, therefore detection sensitivity is high
(b) the standard curve linear dependence of this kit detection 25-OH Vintamin D2 and 25-hydroxyvitamin D3
Height, therefore the testing result degree of accuracy is high
With reference to specific embodiment, the present invention is expanded on further it should be understood that these embodiments are merely to illustrate the present invention
Rather than the experimental method of unreceipted actual conditions in the scope of the present invention the following example is limited, generally according to conventional strip
Part, such as Sambrook et al., molecular cloning：Laboratory manual (New York:Cold Spring Harbor
Laboratory Press, 1989) condition described in, or according to the condition proposed by manufacturer unless otherwise indicated, it is no
Then percentage and number are percentage by weight and parts by weight
Embodiment 1
Human serum sample carries out the detection of 25-OH Vintamin D2 and vitamine D3
First, internal standard extract solution prepares
Take 450 μ L internal standards extract solutions to be diluted with 45mL dilutions, fully mix
Extraction
Take 100 μ L human serums to add 500 μ L internal standard extract solutions respectively, be vortexed 1 minute, 14000 revs/min centrifuge 5 minutes,
400 μ L of supernatant liquid are pipetted into 96 hole reaction plates, puts and is dried up on 96 hole nitrogen evaporators
It is derivative
100 μ L conversion fluid is added into 96 hole reaction plates of drying, after being vortexed 5 minutes, room temperature is placed 1 hour
Redissolve
After adding 50 μ L redissolution liquid, vibrate 10 minutes
Liquid-phase condition
Mobile phase prepares
A phases：1mL Mobile Phase Additives A is taken to be added in the 1000mL aqueous solution
B phases：1mL Mobile Phase Additives A and 1mL Mobile Phase Additives B is taken to be added in methanol respectively
Liquid chromatogram is eluted using gradient mode, and liquid phase chromatogram condition includes：
Chromatographic column：Octadecylsilane chemically bonded silica is filler or suitable person
Chromatographic column column temperature：40℃
Sample size：5μL
Flow velocity：0.5mL/min
Gradient：0-0.6min：Mobile phase B is 70%-100%；0.6-1.2min：Mobile phase B is 100%；1.2-
1.21min：Mobile phase B is 100%-70%；1.21-3.0min：Mobile phase B is 70%
Mass Spectrometry Conditions
The multiple-reaction monitoring ion pair (MRM) of table 1 and corresponding voltage parameter
Other mass spectrometry parameters
Ion gun：Electron spray (ESI) ion gun
Ionizing voltage：5500V
Auxiliary plus hot air temperature：550℃
Atomization gas (GAS1)：60psi
Auxiliary heating gas (GAS2)：60psi
Gas curtain gas (CUR)：20psi
Collision gas (CAD)：4psi
Upper machine testing：
LC-MS instrument parameter is set according to chromatographic condition and Mass Spectrometry Conditions, by the reference substance handled well, quality-control product and inspection
Survey sample solution injection instrument to be detected, and record chromatogram (Fig. 3, Fig. 4 as shown in Figure 1, Figure 2) and tieed up with detection sample 25- hydroxyls
Raw plain D2, the peak area of 25-hydroxyvitamin D3 and Isotopic Internal Standard 25-OH Vintamin D2-d3,25-hydroxyvitamin D3-
D3 peak areas.
Quantitative analysis
The method for drafting of standard curve：Using the sign concentration of 7 reference substances as abscissa (x), with the reality of 7 reference substances
The ratio for detecting peak area and respective internal standard peak area is ordinate (y), draws standard curve.
The fitting of calibration curve equation：Sign concentration (x) is linearly returned with the peak area ratio (y) of 7 reference substances
Regression equation can be obtained by returning：Y=a+bx, wherein y are ordinate, and x is abscissa, and a is intercept, and b is 25- hydroxyls in slope this example
The regression equation of calciferol is y=0.0204x+-0.00107, as shown in Figure 5；The regression equation of 25-hydroxyvitamin D3 is
Y=0.0103x+-0.00658, as shown in Figure 6.
Detect the calculating of sample results：The ratio of the actual peak area and internal standard peak area that detect sample is substituted into above-mentioned mark
Directrix curve equation, the concentration of testing compound in detection sample is calculated, is shown in Table 2-1,2-2.
Table 2-1 25-OH Vintamin D2s
Table 2-2 25-hydroxyvitamin D3s
All it is incorporated as referring in this application in all documents that the present invention refers to, it is independent just as each document
It is incorporated as with reference in addition, it is to be understood that after the above-mentioned instruction content of the present invention has been read, those skilled in the art can like that
To be made various changes or modifications to the present invention, these equivalent form of values equally fall within the model that the application appended claims are limited
Enclose.
Claims (10)
- A kind of 1. high performance liquid chromatography MS detection kit, it is characterised in that including：(1) quality-control product, 25-OH Vintamin D2 and 25-hydroxyvitamin D3 are contained in described quality-control product；(2) Isotopic Internal Standard extract solution, 25-OH Vintamin D2-d3 and 25- hydroxyls are contained in described Isotopic Internal Standard extract solution Base vitamine D3-d3；(3) dilution, described dilution are acetonitrile；(4) conversion fluid, described conversion fluid are PTAD (4- phenyl -1,2,4- triazolines -3,5- diketone)；(5) liquid is redissolved, described redissolution liquid is methanol；(6) Mobile Phase Additives A, described Mobile Phase Additives A are saturated monocarboxylic acid；(7) Mobile Phase Additives B, wherein described Mobile Phase Additives B is C1-C3 amines.
- 2. described detection kit is required according to right 1, it is characterised in that described Mobile Phase Additives B is methylamine.
- 3. detection kit as claimed in claim 1, it is characterised in that the saturated monocarboxylic acid is formic acid, acetic acid, third Acid, butyric acid or its combination.
- 4. detection kit as claimed in claim 3, it is characterised in that the saturated monocarboxylic acid is formic acid.
- 5. detection kit as claimed in claim 1, it is characterised in that the saturated monocarboxylic acid is one of methanol and ethanol Or its combination.
- 6. detection kit as claimed in claim 1, it is characterised in that the saturated monocarboxylic acid is methanol.
- 7. the side of the amount of one or more dihydroxyvitamin D metabolites in taken biological sample is determined by tandem mass spectrometry Method, it is characterised in that methods described includes step：(i) electricity is carried out to one or more hydroxy vitamin D metabolites and internal standard by using electric spray ion source (ESI) From producing one or more hydroxy vitamin D metabolites and the interior target at least one precursor ion respectively；(ii) one kind of precursor ion described in one or more hydroxy vitamin D metabolites and the interior target is produced respectively Or a variety of fragment ions；With(iii) caused one or more hydroxy vitamin D metabolites and described in comparison step (i) or (ii) or both The amount of the one or more ions of interior target is to determine one or more hydroxy-vitamine D generations in the biological sample Thank to the amount of thing；Wherein, methylamine is added in the mobile phase in chromatogram detection process.
- 8. the method for claim 7, it is characterised in that one or more dihydroxyvitamin D metabolites include 25- hydroxyls Calciferol；And the matter of the parent ion of wherein described 25-OH Vintamin D2/lotus ratio is 619.3 ± 0.5.
- 9. the method for claim 7, it is characterised in that one or more dihydroxyvitamin D metabolites include 25- hydroxyls Vitamine D3；And the matter of the parent ion of wherein described 25-hydroxyvitamin D3/lotus ratio is 607.3 ± 0.5.
- 10. the method for claim 8 or 9, it is characterised in that wherein described one or more fragment ions include being selected from matter/lotus Than one or more ions of the ion for 298.3 ± 0.5.
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| CN110849959A (en) * | 2019-08-28 | 2020-02-28 | 重庆同怡生物技术研究院有限公司 | Derivatization reagent using method for vitamin D quantitative detection |
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| CN113640428A (en) * | 2021-08-24 | 2021-11-12 | 青岛惠安康生物工程有限公司 | Liquid chromatography tandem mass spectrometry detection method and kit for 25-hydroxy vitamin D in dried blood tablets |
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