CN106855551B - The analysis method of the relevant important metabolin of glucose metabolism in serum sample - Google Patents
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Abstract
The invention discloses a kind of analysis methods of the relevant important metabolin of glucose metabolism in serum sample, are extracted using methanol, and it is derivative for the triple level four bars mass spectrometer analyses of gas-chromatography-that two steps are carried out after sample freeze-drying.It is detected using multiple-reaction monitoring pattern, for the metabolin of low content, optimization obtains the optimal ion pair of abundance as quota ion pair, improves sensitivity；And for the metabolin of high-content, after optimization, the low ion pair of selection abundance is as quota ion pair, to widen its range of linearity, analysis while to realize high and low abundance metabolin.Analysis method of the invention has many advantages, such as that simple pre-treatment, reproducible, high sensitivity, the range of linearity are wide.
Description
Technical field
It is a kind of based on the triple level four bars matter of gas-chromatography-the present invention relates to analytical chemistry field and biochemical field
The method that spectrum combination multiple-reaction monitoring pattern carries out the relevant important metabolite analysis of glucose metabolism in serum sample.
Background technique
Glucose is the types of transportation of sugar in blood, and main status is occupied in body glycometabolism, is the work that sustains life
Dynamic important substance.Glucose is changed into pyruvic acid by glycolysis and generates energy, and pyruvic acid passes through three under aerobic conditions
Carboxylic acid recycle and oxidative phosphorylation exhaustive oxidation form CO2And H2O generates a large amount of free energys；And it is then converted under anaerobic
Lactic acid.Glucose is not only that body provides a large amount of free energys, and provides for the synthesis of some substances through glycolysis to exhaustive oxidation
Precursor substance, a variety of diseases such as metabolic disorder and cancer, cardiovascular disease, metabolic syndrome, diabetes are closely related.Therefore
The analysis method for establishing the relevant important metabolin of simple, steady, highly sensitive glucose metabolism will be to be metabolized phase with it
The physiology and pathological study of pass provide help.
The relevant important metabolin of glucose metabolism is very big in blood level difference, according to HMDB database
The concentration maximum of the levels range provided in (http://www.hmdb.ca/), correlative metabolites differs 4 orders of magnitude,
It is analyzed and causes very big difficulty.Occur multiple technologies in recent years for the relevant important metabolin of glucose metabolism
Analysis.The problems such as Luo etc. reports the targeting analysis method based on LC-MS, but there are sensitivity and coverages；The report such as Ye
, there is coverage in quasi- targeted approach of the road based on gas chromatography mass spectrometry.In terms of quantitative analysis, usually to glucose and three
Carboxylic acid recycle intermediate product is analyzed respectively.The measurement of glucose mainly has enzyme process, electrochemical process, photochemical method etc.；Tricarboxylic
The method that the quantitative analysis of sour intercycle product is mostly used gas chromatography mass spectrometry, such as Calder ó n-Santiago use chloroform methanol
Water two-phase is extracted, and selects ion scan mode detection, but exist and extract the problems such as complicated, solvent toxicity is big.Gas-chromatography-is triple
Level four bars mass spectrometric hyphenated technique analyzes strong tool as targeting, combines the mass spectrographic choosing of two-stage by gas-chromatography separation
Ion scan is selected, excludes matrix interference to the maximum extent, has many advantages, such as that high sensitivity, the range of linearity are wide；And it there is not yet is based on
The relevant important metabolin of the triple level four bars mass spectrometry multiple-reaction monitoring pattern analysis glucose metabolisms of gas-chromatography-
Relevant report.
Summary of the invention
The present invention is directed to the deficiency of existing method, establishes the triple level four bars mass spectrometry multiple-reaction monitorings of gas-chromatography-
Mode carries out the analysis method of the relevant important metabolin of glucose metabolism, can single injected sampling analyze to obtain grape in serum
The content of the relevant important metabolin of sugared energetic supersession, for the research of related disease metabolism, for the physiology course for understanding body
And occurrence and development mechanism of disease etc. provides foundation.This method has pre-treatment simple, high sensitivity, reproducible, linear model
The advantages that enclosing width.
The technology path that the present invention uses is as follows:
(1) serum sample for saving -80 DEG C thaws, and vortex 10s accurately pipettes 50 μ L, and the methanol that containing the internal standard is added is molten
Liquid 200 μ L, vortex 1min.Internal standard concentration is respectively as follows: lactic acid -3,3,3-d in methanol solution3(100 μ g/mL), succinic acid -2,2,
3,3-d4(0.2 μ g/mL), fumaric acid -2,3-d2(0.1 μ g/mL), citric acid -2,2,4,4-d4(5 μ g/mL), glucose-13C6,
1,2,3,4,5,6,6-d7(150μg/mL).14000rpm is centrifuged 15min at 4 DEG C, and 200 μ L supernatant solutions is taken to be freeze-dried.
(2) 50 μ L methoxy amine aqueous solutions (20mg.ml, pyridine) are added in freeze-drying serum sample, vortex 30s, ultrasonic 1min,
1.5h is reacted in 37 DEG C of water-baths；To the end of reacting, 40 μ LN- methyl-N- (trimethylsilyl) trifluoroacetamides are added, are vortexed
10s reacts 1h in 37 DEG C of water-baths；After the reaction was completed, 14000rpm is centrifuged 10min at 4 DEG C, takes supernatant solution for analyzing.
(3) the triple level four bars mass spectrometry instruments of gas-chromatography-are used for sample analysis.
GC conditions: HP-5MS chromatographic column (30m × 0.25mm × 0.25 μm, Agilent Technologies,
USA).Column temperature uses temperature programming, and 70 DEG C of holdings 1min, 5 DEG C/min rise to 190 DEG C, and 15 DEG C/min rises to 310 DEG C, rear to balance
5min.300 DEG C of injector temperature, sampling volume 1 μ L, split ratio 1:5.Helium (99.9995%, China) is used as carrier gas, flow velocity
1.2mL/min, constant current mode；
Mass Spectrometry Conditions: the source EI, -70eV, transmission line and ion source temperature are 280 DEG C and 230 DEG C respectively.The solvent delay time
5.5min.Collision gas is nitrogen, flow velocity 1.5mL/min；It is helium, flow velocity 2.25mL/min that gas, which is quenched,.Using more reaction prisons
Mode detection is surveyed, for low content metabolin, the parent ion for selecting abundance high carries out daughter ion scanning to it and optimizes collision
Can, select the ion pair that S/N is maximum and specificity is good as quota ion pair, and be aided with qualitative ion pair；For high-content generation
It thanks object (lactic acid, glucose), the parent ion for selecting abundance low, daughter ion scans and optimizes impact energy, selects low-abundance ion
To as quota ion pair, and it is aided with qualitative ion pair.Subordinate list 1 be optimization after obtain metabolin quota ion pair, it is qualitative from
Son is right, and its corresponding impact energy information.
(4) mass spectrometric data is exported with Masshunter Quantitative Analysis Software, using internal standard method
Quantitative analysis is carried out to metabolin.
This method uses methanol onestep extraction, extracts relative to chloroform methanol water two-phase, and this method is easy to operate, repeated
Good and solvent toxicity is small；And it is detected using the triple level four bars mass spectrum multiple-reaction monitoring patterns of gas-chromatography-, anti-interference energy
Power is strong, high sensitivity, for low content metabolism analyte detection limit in 0.17-2.13ng/mL；It is excellent by ion pair selection and impact energy
Change, high low content metabolin may be implemented while testing and analyzing.
Detailed description of the invention
Fig. 1 is the relevant important metabolin of glucose metabolism and interior target total ion current in normal person's serum sample
Figure.
Fig. 2 is the relevant important metabolin of glucose metabolism and interior target quota ion pair in normal person's serum sample
Extract flow graph.
Specific embodiment
Elaborate with reference to the accompanying drawing to the embodiment of the present invention: embodiment is based on the technical solution of the present invention
Under implemented, the detailed implementation method and specific operation process are given, but protection scope of the present invention be not limited to it is following
Embodiment.
Embodiment one
It is relevant important based on glucose metabolism in the triple level four bars mass spectrometry detection serum samples of gas-chromatography-
The evaluation of metabolin method
With reference to HMDB database (http://www.hmdb.ca/), if different age people blood-sugar content range is in 1100-
16440 μM, i.e. 198.2-2961.8 μ g/mL.Mixed mark solution, concentration are prepared according to the reference concentration range of metabolin in database
Respectively pyruvic acid (800.0 μ g/mL), lactic acid (4000 μ g/mL), succinic acid (800.0 μ g/mL), fumaric acid (800.0 μ g/
ML), malic acid (800.0 μ g/mL), 2- hydroxyl glutaric acid (800.0 μ g/mL), 2-oxoglutaric acid (800.0 μ g/mL), aconitic acid
(800.0 μ g/mL), citric acid (800.0 μ g/mL), isocitric acid (800.0 μ g/mL), glucose (4000 μ g/mL) use pure water
By mixed mark solution dilute respectively 1.33 times, 1.6 times, 2.67 times, 4 times, 8 times, 40 times, 80 times, 400 times, 800 times, 4000 times,
8000 times, 20000 times, 40000 times, 100000 times, 200000 times, 500000 times, 1000000 times, 2500000 times obtain difference
The mixed mark solution of concentration.Each 50 μ L of mixed mark solution for taking various concentration is separately added into the methanol solution of 200 μ L containing the internal standards, is vortexed
1min；Internal standard concentration is respectively as follows: lactic acid -3,3,3-d in methanol solution3(100 μ g/mL), succinic acid -2,2,3,3-d4(0.2μg/
ML), fumaric acid -2,3-d2(0.1 μ g/mL), citric acid -2,2,4,4-d4(5 μ g/mL), glucose-13C6,1,2,3,4,5,6,
6-d7(150μg/mL).14000rpm is centrifuged 15min at 4 DEG C, and 200 μ L supernatant solutions is taken to be freeze-dried.
50 μ L methoxy amine aqueous solutions (20mg/ml pyridine), vortex 30s, ultrasonic 1min, 37 DEG C of water-baths are added in freeze-drying sample
Middle reaction 1.5h；To the end of reacting, it is added 40 μ L N- methyl-N- (trimethylsilyl) trifluoroacetamides, vortex 10s, 37 DEG C
1h is reacted in water-bath；After the reaction was completed, 14000rpm is centrifuged 10min at 4 DEG C, takes supernatant solution for gas-chromatography-triple four
Grade bar mass spectrometry instrument analysis.
GC conditions: HP-5MS chromatographic column (30m × 0.25mm × 0.25 μm, Agilent Technologies,
USA)；Column temperature uses temperature programming, and 70 DEG C of holdings 1min, 5 DEG C/min rise to 190 DEG C, and 15 DEG C/min rises to 310 DEG C, rear to balance
5min；300 DEG C of injector temperature, sampling volume 1 μ L, split ratio 1:5；Helium (99.9995%, China) is used as carrier gas, flow velocity
1.2mL/min, constant current mode.Mass Spectrometry Conditions: the source EI, -70eV, transmission line and ion source temperature are 280 DEG C and 230 DEG C respectively.
Solvent delay time 5.5min；Collision gas is nitrogen, flow velocity 1.5mL/min；It is helium, flow velocity 2.25mL/min that gas, which is quenched,.
It is less than or equal to the metabolin of 100 μ g/mL for content, selects the higher candidate parent ion of response in not syn-collision
(CE=0-35V) carries out daughter ion scanning under the conditions of energy, selects the highest ion pair of signal-to-noise ratio as quota ion pair；And for
Content is higher than the metabolin of 100 μ g/mL, selects lower candidate parent ion (CE=0- under the conditions of different impact energies of response
35V) carry out daughter ion scanning, the ion pair for selecting the range of linearity wide as quota ion pair, finally obtain 11 kinds of metabolins and
Target quota ion pair, qualitative ion pair in its 5 kinds, and its corresponding impact energy information see attached list 1.It is determined according to subordinate list 1
Mass Spectrometry Conditions carry out the linear analysis of method using the mixed mark solution of various concentration, obtain the range of linearity and linear phase of metabolin
Close coefficients R21 is seen attached list, analysis is all satisfied and requires.
The rate of recovery for having investigated method, the serum sample that -80 DEG C are saved thaw, and vortex 10s accurately pipettes 50 μ L respectively
Serum sample carries out blank and recovery of standard addition analysis.10 μ L of methanol, recovery of standard addition is added using serum in blank control sample
Sample is then separately added into the mixed mark 10 μ L of solution of basic, normal, high concentration in serum sample, and above-mentioned solution adds the methanol of containing the internal standard
Solution 190 μ L, vortex 1min, investigate basic, normal, high concentration recovery of standard addition.Blank and recovery of standard addition are repeated 6 times.In it is dense
The mixed mark solution concentration of degree is respectively as follows: pyruvic acid (17.5 μ g/mL), lactic acid (1100 μ g/mL), succinic acid (4.0 μ g/mL), rich horse
Sour (1.25 μ g/mL), malic acid (3.0 μ g/mL), 2- hydroxyl glutaric acid (1.75 μ g/mL), 2-oxoglutaric acid (15.0 μ g/mL),
Aconitic acid (1.75 μ g/mL), citric acid (80.0 μ g/mL), isocitric acid (2.5 μ g/mL), glucose (2000 μ g/mL)；Low,
The concentration of the mixed mark solution of high concentration is 0.8 times, 1.2 times of the mixed mark solution concentration of middle concentration respectively.Internal standard concentration in methanol solution
It is respectively as follows: lactic acid -3,3,3-d3(100 μ g/mL), succinic acid -2,2,3,3-d4(0.2 μ g/mL), fumaric acid -2,3-d2(0.1μ
G/mL), citric acid -2,2,4,4-d4(5 μ g/mL), glucose-13C6,1,2,3,4,5,6,6-d7(150μg/mL).At 4 DEG C
14000rpm is centrifuged 15min, and 200 μ L supernatant solutions is taken to be freeze-dried.After derivative by analysis and calculate, in basic, normal, high concentration
Recovery of standard addition in 78.1-112.5%, meet analysis and require；And each parallel 6 parts of blank, basic, normal, high mark-on sample
RSD is reproducible within 10%.
The mixed mark solution of middle concentration is diluted into 50 times, 100 times, 500 times, 1000 times, 10000 times, 50000 times respectively, is respectively taken
200 μ L methanol are added in 50 μ L, are vortexed after mixing and 200 μ L solution is taken to be lyophilized, then deriveding analysis；With S/N under low consistency conditions
=3 detection limits for obtaining low content metabolin see attached list 1 (in addition to lactic acid, glucose) within the scope of 0.17-2.13ng/mL, remove
Aconitic acid is with the sensitivity of Salbutamol Selected Ion Monitoring method reported in the literature based on gas chromatography mass spectrometry suitable, the metabolism of remaining low content
The sensitivity of object improves 3.7-58.3 times.
Embodiment two
The relevant important metabolism analyte detection of normal human serum sample glucose energetic supersession
The normal human serum sample that -80 DEG C are saved thaws, and vortex 10s accurately pipettes 50 μ L, the methanol of containing the internal standard is added
Solution 200 μ L, vortex 1min.Internal standard concentration is respectively as follows: lactic acid -3,3,3-d in methanol solution3(100 μ g/mL), succinic acid -2,
2,3,3-d4(0.2 μ g/mL), fumaric acid -2,3-d2(0.1 μ g/mL), citric acid -2,2,4,4-d4(5 μ g/mL), glucose-13C6,1,2,3,4,5,6,6-d7(150μg/mL).14000rpm is centrifuged 15min at 4 DEG C, takes the freezing of 200 μ L supernatant solutions dry
It is dry.50 μ L methoxy amine aqueous solutions (20mg.ml, pyridine) are added in freeze-drying sample, and vortex 30s, ultrasonic 1min are anti-in 37 DEG C of water-baths
Answer 1.5h；To the end of reacting, 40 μ L N- methyl-N- (trimethylsilyl) trifluoroacetamides, vortex 10s, 37 DEG C of water-baths are added
Middle reaction 1h；After the reaction was completed, 14000rpm is centrifuged 10min at 4 DEG C, and supernatant is taken to carry out the triple level four bars mass spectrums of gas-chromatography-
It is combined instrument analysis.
GC conditions: HP-5MS chromatographic column (30m × 0.25mm × 0.25 μm, Agilent Technologies,
USA).Column temperature uses temperature programming, and 70 DEG C of holdings 1min, 5 DEG C/min rise to 190 DEG C, and 15 DEG C/min rises to 310 DEG C, rear to balance
5min.300 DEG C of injector temperature, sampling volume 1 μ L, split ratio 1:5.Helium (99.9995%, China) is used as carrier gas, flow velocity
1.2mL/min, constant current mode.Mass Spectrometry Conditions: the source EI, -70eV, transmission line and ion source temperature are 280 DEG C and 230 DEG C respectively.
Solvent delay time 5.5min.Collision gas is nitrogen, flow velocity 1.5mL/min；It is helium, flow velocity 2.25mL/min that gas, which is quenched,.
It is detected using multiple-reaction monitoring pattern.
Using above-mentioned analysis method, obtain the relevant important metabolin of glucose metabolism in normal human serum sample and
Interior target total ion current figure, which is shown in Fig. 1 and extracts ion flow graph, sees Fig. 2.Using inner mark method ration, grape in normal human serum sample
The content difference of the relevant important metabolin of sugared energetic supersession is as follows: about 0.92 μ g/mL of pyruvic acid, about 149.67 μ g/mL of lactic acid,
About 0.20 μ g/mL of succinic acid, about 0.08 μ g/mL of fumaric acid, about 0.08 μ g/ of about 0.36 μ g/mL, 2- hydroxyl glutaric acid of malic acid
ML, about 0.07 μ g/mL of 2-oxoglutaric acid, about 0.15 μ g/mL of aconitic acid, about 12.99 μ g/mL of citric acid, about 0.37 μ of isocitric acid
G/mL, about 737.91 μ g/mL of glucose.
Invention effect:
The present invention uses the single-phase extraction of methanol, carries out glucose metabolism in conjunction with triple level four bars multiple-reaction monitoring patterns
The highly sensitive detection and analysis of relevant important metabolin.Compared with existing method reported in the literature, there is following advantage:
1. the present invention carries out glucose metabolism correlation in blood sample sample using triple level four bars multiple-reaction monitoring patterns
Important metabolin highly sensitive detection and analysis, have no the document report of the detection pattern before；
2. realizing the single injected sampling same time-division of high low content metabolin by the selection of ion pair and the optimization of impact energy
Analysis；
3. being detected using multiple-reaction monitoring pattern, interference is significantly reduced, the glucose energy generation of low content is realized
The highly sensitive detection for thanking to relevant important metabolin, in addition to aconitic acid is suitable with sensitivity reported in the literature, remaining metabolin phase
3.7-58.3 times is improved for document report sensitivity.
Subordinate list 1
1: using fumaric acid -2,3-d2Correction；2: using lactic acid -3,3,3-d3Correction；3: using succinic acid -2,2,3,3-
d4Correction；4: using citric acid -2,2,4,4-d4Correction；5: using glucose-13C6,1,2,3,4,5,6,6-d7Correction.
Claims (4)
1. the analysis method of the relevant important metabolin of glucose metabolism in serum sample, which is characterized in that comprising following
Step:
(1) the extraction solution of containing the internal standard is added in serum sample, is vortexed and mixes, be then centrifuged for, quantitatively pipette supernatant solution, juxtaposition
It is freeze-dried in freeze dryer；
(2) methoxy amine aqueous solution is added in the sample after freeze-drying, dissolves and mixes to metabolin, it is anti-that heating water bath carries out oximate
It answers；N- methyl-N- (trimethylsilyl) trifluoroacetamide is added, is vortexed and mixes, heating water bath carries out Silanization reaction；To
After reaction, low-temperature and high-speed is centrifuged, and takes supernatant solution for analyzing；
(3) sample analysis is carried out using the multiple-reaction monitoring pattern of the triple level four bars mass spectrometries of gas-chromatography-, it is low for content
In or equal to 100 μ g/mL metabolin, select higher candidate parent ion CE=0-35V under the conditions of different impact energies of response
Daughter ion scanning is carried out, selects the highest ion pair of signal-to-noise ratio as quota ion pair；And for content higher than 100 μ g/mL's
Metabolin selects lower candidate parent ion CE=0-35V under the conditions of different impact energies of response and carries out daughter ion scanning, selection
The wide ion pair of the range of linearity realizes that concentration maximum in serum differs the same of the metabolin of 4 orders of magnitude as quota ion pair
When test and analyze；
(4) quantitative analysis is carried out to metabolin using internal standard method；
Internal standard concentration is respectively as follows: the lactic acid -3,3,3-d that concentration is 50-250 μ g/mL in the extraction solution of the containing the internal standard3, dense
Degree is the succinic acid -2,2,3,3-d of 0.1-2.0 μ g/mL4, concentration is fumaric acid -2,3-d of 0.1-2.0 μ g/mL2, concentration is
Citric acid-the 2,2,4,4-d of 1.0-10 μ g/mL4, concentration is the glucose-of 100-500 μ g/mL13C6,1,2,3,4,5,6,
6-d7；
20-200 μ L methoxy amine aqueous solution is added in the step (2) in freeze-drying sample, the methoxy amine aqueous solution is molten with pyridine
Agent, methoxy amine concentration are 20 mg/mL, vortex 30-120 s, ultrasonic 1-15 min, 37-40o1.5-2 h is reacted in C water-bath；
To the end of reacting, it is added 16-160 μ L N- methyl-N- (trimethylsilyl) trifluoroacetamide, vortex 10-30 s, 37oC
0.5-1 h is reacted in water-bath；After the reaction was completed, 4-25o12000-14000 rpm is centrifuged 10-15 min under C, takes supernatant solution
For analyzing；
Sample analysis is carried out using the multiple-reaction monitoring pattern of the triple level four bars mass spectrometries of gas-chromatography-in the step (3)；
GC conditions: HP-5 MS chromatographic column, design parameter are mm × 0.25 μm 30 m × 0.25, Agilent
Technologies, USA；Column temperature use temperature programming, 70oC keep 1 min, 5oC/min rises to 190oC, 15oC/min
Rise to 310oC, it is rear to balance 5 min；Injector temperature 300oC, sampling volume 1 μ L, split ratio 1:5；Purity is 99.9995%,
In domestic helium as carrier gas, 1.2 mL/min of flow velocity, constant current mode；
Mass Spectrometry Conditions: the source EI, -70 eV, transmission line and ion source temperature are 280 respectivelyoC and 230oC, solvent delay time 5.5
min；Collision gas is nitrogen, 1.5 mL/min of flow velocity；It is helium that gas, which is quenched, and flow velocity is 2.25 mL/min.
2. analysis method according to claim 1, which is characterized in that step (1) quantitatively pipettes 20-200 μ L serum sample
This, is added methanol solution 80-800 μ L, vortex the 0.5-2 min of containing the internal standard； 4-25o12000-14000 rpm is centrifuged under C
10-20 min takes 80-800 μ L supernatant solution to be freeze-dried.
3. analysis method according to claim 1, which is characterized in that detected using multiple-reaction monitoring pattern, for content
Less than or equal to the metabolin of 100 μ g/mL, selects the higher candidate parent ion of response and carry out son under the conditions of different impact energies
Ion scan selects the highest ion pair of signal-to-noise ratio as quota ion pair；And it is higher than the metabolism of 100 μ g/mL for content
Object selects the lower candidate parent ion of response and carries out daughter ion scanning under the conditions of different impact energies, selects the range of linearity wide
Ion pair is aided with qualitative ion pair as quota ion pair.
4. analysis method according to claim 1, which is characterized in that inner mark method ration is used in step (4), according to linear
Quantitation curves are calculated.
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