CN110161140A - The Liquid Chromatography-Tandem Mass Spectrometry method of urine citric acid and oxalic acid content is detected simultaneously - Google Patents
The Liquid Chromatography-Tandem Mass Spectrometry method of urine citric acid and oxalic acid content is detected simultaneously Download PDFInfo
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Abstract
The present invention provides Liquid Chromatography-Tandem Mass Spectrometry method that is a kind of while detecting urine citric acid and oxalic acid content, including preparation test sample and ultra performance liquid chromatography-tandem mass spectrometry detection；Sample preparation is carried out using Solid Phase Extraction (SPE) mode, urine specimen is diluted with water first, then the isotope labelling internal standard of oxalic acid and citric acid is added, the SPE plate after overactivation is added after mixing, then it is eluted by the alkaline solution of ammonium hydroxide is added, and certain density aqueous formic acid is added in sample after collection, keep its acid condition, the sample prepared is entered into chromatographic mass spectrometry system by chromatograph sampling later, passes through the initial gross separation of chromatographic column；Into in mass spectrum, citric acid and oxalic acid are detected further according to different mass-to-charge ratioes is generated in mass spectrum.This method pre-treatment is simple, is not required to that derivative, urine sample dosage is less, can quick, special detection urine oxalic acid and citric acid content.
Description
Technical field
The present invention relates to the detection methods of citric acid in urine and oxalic acid content, and in particular to uses liquid chromatography tandem matter
The method that spectral technology detects urine citric acid and oxalic acid content simultaneously.
Background technique
Stone in urinary system is one of common disease of Urology Surgery, occupies first place in Urology Surgery inpatient.According to document
(Wang W,Fan J,Huang G,Li J,Zhu X,Tian Y,Su L(2017)Prevalence of kidney stones
In mainland China:a systematic review.Sci Rep, 7:41630) report 1991-2000 years, 2001-
The prevalence rate of 2010 and 2011 annual calculus is respectively 5.95%, 8.86% and 10.63%, in the trend of rising appreciably.Uropoiesis
Tying stone high recurrence rate prevents according to European stone in urinary system and assesses guide (EAU guidelines for
Urolithiasis) report: the risk that a kind of doctor forms stone in urinary system is 5%-10%, if not carrying out to calculus patient pre-
Anti- property intervention, 5 years recurrence rates are up to 80-90% up to 50%, 10 year recurrence rate, and the good hair age of calculus is male at 30-50 years old
The ratio between female about 2-3:1.All these Notes of Key Datas we, stone in urinary system is as illness rate, a high recurrence rate, disease incidence
Increase year by year, and main labour is in the disease of high risk, is a public health to human health with significant impact
Problem can not be ignored.
Hyperoxaluria is the Important cause of disease of the calcinm oxalate calculus in stone in urinary system, and citric acid is stone in urinary system
Important inhibiting factor.The most common with calcinm oxalate calculus in China, urinary calculi, the hyperoxaluria of Oxalate metabolism caused by abnormal exists
Be of great significance on calculus, citric acid radical ion can be coordinated with calcium ion, inhibit the urinary calculis mineral such as calcium oxalate at
Core and growth with alkalized urine, can be such that the solubility of acid class calculus such as calculus urate and cystine stone increases.It is accurate to survey
Determine the oxalic acid and citric acid in urine, it can be to provide support by diet intervention or clinical prevention.
The method of measurement oxalic acid and citric acid mainly has colorimetric method, high performance liquid chromatography and the chromatography of ions at present.
Citric acid or oxalic acid content in colorimetric method for determining urine, method sensitivity is low, poor specificity, can not be to urine sample
In micro citric acid carry out accurate quantitative analysis, and oxalic acid and citric acid can not be measured simultaneously.
The method of high effective liquid chromatography for measuring oxalic acid generally requires to come out the oxalic acid precipitation in sample in preceding processing
It can measure, its content can not then be measured simultaneously for the citric acid that cannot be precipitated in sample.
There are also some researchs to use the chromatography of ions and capillary electrophoresis technique, can measure simultaneously oxalic acid in urine and
Citric acid, but be restricted at home because instrument is not easy acquisition, and the quasi-instrument is without medical instrument registration certificate.
Consulting literatures discovery has the method report (east that citric acid or oxalic acid are measured using Liquid Chromatography-Tandem Mass Spectrometry method
It is clean etc., application of the liquid chromatography-mass spectrography serial connection technology in urine citric acid assay；Chinese Medical Journal, 2017,97:
3471-3474；East is clean etc., the meaning of liquid chromatography-mass spectrography serial connection technology quantitative determination urine medium-height grass acid content, and Chinese medical is miscellaneous
Will, 2017,97:2043-2046), but it is not yet found that effect liquid phase chromatogram method tandem mass spectrometry measures oxalate crystal growth in healthy urine simultaneously
With the method and kit of citric acid.
Summary of the invention
To overcome the shortcomings of the existing technology, simple, same using less sample size, pre-treating method present invention aims at establishing
When measurement urine in citric acid and oxalic acid Liquid Chromatography-Tandem Mass Spectrometry method, and prepare its corresponding kit.
Specifically, the present invention provides while detecting the Liquid Chromatography-Tandem Mass Spectrometry side of urine citric acid and oxalic acid content
Method, including preparation test sample and ultra performance liquid chromatography-tandem mass spectrometry detection.
Wherein, preparation test sample method includes: to take urine sample to be measured, and oxalic acid-is added13C2As the internal standard of oxalic acid,
Citric acid-13C6Internal standard as citric acid；Upper 96 orifice plate of weak cation exchange after 2% aqueous formic acid mixes is added, with 5%
Ammonium hydroxide elution, collects eluent, 5% ammonium hydroxide is added, as test sample.
Specifically, preparation test sample method includes: to take 30 μ L samples or calibration object to 5mL glass tube, and it is same that 20 μ L are added
2% aqueous formic acid of 1mL, mixing concussion is added in the plain internal standard in position；Loading: on into the sample well of 96 orifice plate of weak cation exchange
750 μ L of sample, is slowly blown down with positive pressure of nitrogen, and 200 μ L pure water are being added, are being blown down with positive pressure of nitrogen；Elution: it is added into sample well
80 μ L, 5% ammonium hydroxide is slowly blown down with positive pressure of nitrogen, collects eluent, and 5 μ L, 5% ammonium hydroxide is added, and waits examination with computer.
Wherein, 96 orifice plate of weak cation exchange need to activate in advance, method particularly includes: 200 μ L methanol are added into sample well,
It is blown down with positive pressure of nitrogen, then 200 μ L pure water is added into sample well, blown down with positive pressure of nitrogen.
Chromatographic condition is as follows:
Chromatographic column: T3 chromatographic column (1.8 μm, 2.1 × 100mm)；
Mobile phase A: chromatographic grade acetonitrile；Mobile phase B: the aqueous solution containing 0.3% formic acid；According to the form below carries out gradient elution:
| Time/min | % mobile phase A | % Mobile phase B |
| Starting | 1.0 | 99 |
| 1 | 1.0 | 99 |
| 2 | 90 | 10 |
| 3 | 90 | 10 |
| 4 | 1.0 | 99 |
Flow velocity is 0.3ml/min；
5 μ L of sample volume；
Mass Spectrometry Conditions are as follows:
Mass spectrum selection multi-ion monitoring reaction pattern, negative ion mode, electrospray ionisation, 300-600 DEG C of ion source temperature,
Preferably 500 DEG C, the ion pair specifically monitored and collision energy (CE), remove cluster voltage (DP) etc. and see the table below (DP, EP, CE,
CXP is not fixed, and is changed according to instrument):
The above method further includes, using the oxalic acid-of stable isotope labeling13C2Internal standard as oxalic acid；Citric acid-13C6
Internal standard as citric acid.By preparing a series of standard items of various concentrations, standard curve is made, is with concentration of standard solution
The ratio of X-axis, standard and internal standard peak area is Y-axis, carries out linear regression analysis, obtains regression equation through " 1/X " weight.By sample
In ingredient to be measured and its internal standard peak area ratio substitute into calibration curve equation, calculate the concentration of each ingredient to be measured in urine sample.Sample
The concentration of ingredient to be measured is proportional in the ratio and sample of this detection signal strength and Isotopic Internal Standard.
The present invention is the detection specific designs according to Liquid Chromatography-Tandem Mass Spectrometry, in conjunction with the molecule of citric acid and oxalic acid
Amount, the two generated in mass spectrum special mass/charge ratio (mass-to-charge ratio) and the polarity difference in chromatography be monitored and
Separation.
Sample preparation is carried out using Solid Phase Extraction (SPE) mode, is first diluted urine specimen with water, is then added
The SPE plate after overactivation is added in the isotope labelling internal standard of oxalic acid and citric acid after mixing, then by ammonium hydroxide is added
Alkaline solution eluted, and certain density aqueous formic acid is added in sample after collection, keeps its acid condition,
The sample prepared is entered into chromatographic mass spectrometry system by chromatograph sampling later, passes through the initial gross separation of chromatographic column；Into matter
In spectrum, citric acid and oxalic acid are detected further according to different mass-to-charge ratioes is generated in mass spectrum.
Based on the above method, the present invention also provides one kind to detect urine citron for Liquid Chromatography-Tandem Mass Spectrometry method simultaneously
The kit of acid and oxalic acid content, comprising: weak anionic exchanges 96 orifice plates, sample preparation liquid, calibration solution and instrument and analyzes liquid；
Wherein, sample preparation liquid includes: pure water；Concentration is 1%~10% aqueous formic acid, and preferably 2% formic acid is water-soluble
Liquid；Concentration is 1%~20% aqueous formic acid, preferably turns to 10% aqueous formic acid；Concentration is 0.1%~10% ammonium hydroxide, excellent
It is selected as 5% ammonium hydroxide；Hplc grade methanol；Isotopic Internal Standard；
The Isotopic Internal Standard contains: oxalic acid-13C2: concentration is 200-1000 μm of ol/L, preferably 500 μm of ol/L；Citron
Acid-13C6: concentration is 10-1000 μm of ol/L, preferably 500 μm of ol/L；
Calibrate solution: concentration of oxalic acid are as follows: 25 μm of ol/L-2000 μm of ol/L；Citron acid concentration range is 50 μm of ol/L-4000
μmol/L；
It is mobile phase A: chromatographic grade acetonitrile that instrument, which analyzes liquid,；Mobile phase B: the aqueous solution containing 0.3% formic acid.
The method that the present invention establishes Liquid Chromatography-Tandem Mass Spectrometry measurement oxalic acid and citric acid, this method sample pre-treatments letter
It is single, be not required to that derivative, urine sample dosage is less, can quick, special detection urine oxalic acid and citric acid content.
Detailed description of the invention
Fig. 1 is that embodiment 1 detects obtained typical spectrogram.
Fig. 2 indicates 1 oxalic acid of embodiment and the linear test result of citric acid.
Fig. 3 indicates 1 experimental result of comparative example.
Fig. 4 indicates 2 experimental result of comparative example.
Fig. 5 indicates 3 experimental result of comparative example.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..It is not specified in embodiment specific
Technology or conditions person, described technology or conditions according to the literature in the art, or carried out according to product description.It is used
Production firm person is not specified in reagent or instrument, is the conventional products that can be commercially available by regular distributor.
Instrument and reagent used below:
High performance liquid chromatography-tandem mass instrument: Waters Xevo TQ-S.
Isotopic Internal Standard contains: oxalic acid-13C2: concentration is 500 μm of ol/L；Citric acid-13C6: concentration is 500 μm of ol/L；
2% aqueous formic acid；10% aqueous formic acid, 5% ammonium hydroxide；Hplc grade methanol.
Embodiment 1
Preparation test sample: it takes 30 μ L samples or calibration object to 5mL glass tube, 20 μ L Isotopic Internal Standards is added, are added
2% aqueous formic acid of 1.5mL, mixing concussion；Loading: the 750 μ L of loading into the sample well of 96 orifice plate of weak cation exchange is used
Positive pressure of nitrogen is slowly blown down, and 200 μ L pure water are being added, are being blown down with positive pressure of nitrogen.Elution: 80 μ L, 5% ammonia is added into sample well
Water is slowly blown down with positive pressure of nitrogen, collects eluent, and 5 μ L, 5% ammonium hydroxide is added, and waits examination with computer.
Wherein, 96 orifice plate of weak cation exchange need to activate in advance, method particularly includes: 200 μ L methanol are added into sample well,
It is blown down with positive pressure of nitrogen, then 200 μ L pure water is added into sample well, blown down with positive pressure of nitrogen.
Chromatographic condition is as follows:
Chromatographic column: T3 chromatographic column (1.8 μm, 2.1*100mm)；
Mobile phase A: chromatographic grade acetonitrile；Mobile phase B: the aqueous solution containing 0.3% formic acid；According to the form below carries out gradient elution:
| Time | Flow velocity | % mobile phase A | % Mobile phase B |
| Starting | 0.3 | 1.0 | 99 |
| 1 | 0.3 | 1.0 | 99 |
| 2 | 0.3 | 90 | 10 |
| 3 | 0.3 | 90 | 10 |
| 4 | 0.3 | 1.0 | 99 |
5 μ L of sample volume；
Mass Spectrometry Conditions are as follows:
Mass spectrum selection multi-ion monitoring reaction pattern, negative ion mode, electrospray ionisation, 500 DEG C of ion source temperature, specifically
The ion pair and collision energy (CE) of monitoring remove cluster voltage (DP) etc. and see the table below that (DP, EP, CE, CXP are not fixed, according to instrument
Changed):
The typical spectrogram detected is shown in Fig. 1.The result shows that peak shape is well-symbolized, peak shape is narrow, and analysis time is only
4min, the noiseless peak in determinand peak periphery.
Oxalic acid and the linear test result of citric acid are shown in Fig. 2.Oxalic acid and citric acid are linearly all larger than 0.999.
The rate of recovery and accuracy result of this method see the table below, it is seen that the rate of recovery of this method 92.56%~
112.49%, and expected results deviation is within 15%.
The rate of recovery and accuracy
Studies have shown that formic acid concn or ammonia concn different when different in mobile phase pH value and elution samples,
Peak shape may be seriously affected.The present invention has carried out detailed optimization to different acid base concentrations.
Comparative example 1
Inappropriate ammonia concn is added, citric acid peak shape bifurcated: the difference with embodiment 1 is only that, before sample
It manages in elution step, the concentration of ammonium hydroxide is adjusted to 1%.Testing result is shown in Fig. 3.As a result as it can be seen that citric acid peak shape bifurcated.Show
Inappropriate ammonia concn may cause citric acid peak shape bifurcated.
Comparative example 2
Different formic acid concns may will affect the peak shape of oxalic acid: the difference with embodiment 1 is only that: last in preceding processing
In one step, the concentration of formic acid is adjusted to 0.5%.Testing result is shown in Fig. 4.As a result as it can be seen that oxalic acid peak shape is deteriorated.Show not conforming to
Suitable formic acid concn may cause the hangover of oxalic acid peak shape.
Comparative example 3
According to application (east clean etc.) of the document liquid chromatography-mass spectrography serial connection technology in urine citric acid assay；In
Magnificent medical journal, 2017,97:3471-3474) method recorded in.As a result see Fig. 5, it is seen that citric acid peak shape: symmetry is poor,
Peak is wide.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, fall within the scope of the claimed invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. a kind of Liquid Chromatography-Tandem Mass Spectrometry method for detecting urine citric acid and oxalic acid content simultaneously, which is characterized in that including
Prepare test sample and ultra performance liquid chromatography-tandem mass spectrometry detection；
Wherein, the method for the preparation test sample includes: to take urine sample to be measured, and oxalic acid-is added13C2As in oxalic acid
Mark, citric acid-13C6Internal standard as citric acid；Upper 96 orifice plate of weak cation exchange after 2% aqueous formic acid mixes is added, uses
The elution of 5% ammonium hydroxide, collects eluent, 5% ammonium hydroxide is added, as test sample.
2. the method according to claim 1, wherein the preparation test sample method includes: to take 30 μ L samples
Or calibration object is added 20 μ L Isotopic Internal Standards, 1mL2% aqueous formic acid, mixing concussion is added to 5mL glass tube；Loading: to
750 μ L of loading in the sample well of 96 orifice plate of weak cation exchange, is slowly blown down with positive pressure of nitrogen, and 200 μ L pure water are being added, are using nitrogen
Gas positive pressure is blown down；Elution: 80 μ L5% ammonium hydroxide being added into sample well, are slowly blown down with positive pressure of nitrogen, collect eluent, are added 5
μ L5% ammonium hydroxide waits examination with computer；
The Isotopic Internal Standard contains: oxalic acid-13C2: concentration is 200-1000 μm of ol/L；Citric acid-13C6: concentration 10-1000
μmol/L。
3. according to the method described in claim 2, it is characterized in that, the Isotopic Internal Standard contains: oxalic acid-13C2: concentration is
500μmol/L；Citric acid-13C6: concentration is 500 μm of ol/L.
4. method according to claim 1-3, which is characterized in that chromatographic condition is as follows:
Mobile phase A: chromatographic grade acetonitrile；Mobile phase B: the aqueous solution containing 0.3% formic acid；According to the form below carries out gradient elution:
5. method according to claim 1-4, which is characterized in that chromatographic column used is T3 chromatographic column.
6. method according to claim 1-5, which is characterized in that flow rate of mobile phase is 0.3ml/ in chromatographic condition
Sample volume is 5 μ L in min and/or liquid phase chromatogram condition.
7. method according to claim 1-6, which is characterized in that Mass Spectrometry Conditions are as follows:
Mass spectrum selection multi-ion monitoring reaction pattern, negative ion mode, electrospray ionisation, 300-600 DEG C of ion source temperature, specifically
The ion pair and collision energy of monitoring are as follows:
8. method according to claim 1-7, which is characterized in that further include the grass using stable isotope labeling
Acid-13C2Internal standard as oxalic acid；Citric acid-13C6Internal standard as citric acid；By a series of standard for preparing various concentrations
Product make standard curve, and using concentration of standard solution as X-axis, the ratio of standard and internal standard peak area is Y-axis, carry out linear regression
Analysis, obtains regression equation through " 1/X " weight；Ingredient to be measured in sample and its internal standard peak area ratio are substituted into calibration curve equation,
Calculate the concentration of each ingredient to be measured in urine sample.
9. a kind of kit for detecting urine citric acid and oxalic acid content simultaneously for Liquid Chromatography-Tandem Mass Spectrometry method, feature
It is, comprising: weak anionic exchanges 96 orifice plates, sample preparation liquid, calibration solution and instrument and analyzes liquid；
Wherein, sample preparation liquid includes: pure water；Concentration is 1%~10% aqueous formic acid, preferably 2% aqueous formic acid；It is dense
Degree is 1%~20% aqueous formic acid, this reagent is optimized for 10% aqueous formic acid；Concentration is 0.1%~10% ammonium hydroxide, preferably
For 5% ammonium hydroxide；Hplc grade methanol；Isotopic Internal Standard；
The Isotopic Internal Standard contains: oxalic acid-13C2: concentration is 200-1000 μm of ol/L；Citric acid-13C6: concentration 10-1000
μmol/L；
Calibrate solution: concentration of oxalic acid are as follows: 25 μm of ol/L-2000 μm of ol/L；Citron acid concentration range is 50 μm of ol/L-4000 μ
mol/L；
It is mobile phase A: chromatographic grade acetonitrile that instrument, which analyzes liquid,；Mobile phase B: the aqueous solution containing 0.3% formic acid.
10. kit according to claim 9, which is characterized in that the Isotopic Internal Standard contains: oxalic acid-13C2: concentration
For 500 μm of ol/L；Citric acid-13C6: concentration is 500 μm of ol/L.
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| CN110988155A (en) * | 2019-11-15 | 2020-04-10 | 天津市海诺德工贸有限公司 | High performance liquid chromatography for detecting citrate content in hemodialysis solution |
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Application publication date: 20190823 |