CN113588818B - Method for measuring content of acanthopanax bark glycoside M in SD rat plasma - Google Patents
Method for measuring content of acanthopanax bark glycoside M in SD rat plasma Download PDFInfo
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Abstract
The invention discloses a method for measuring the content of acanthopanax bark glycoside M in SD rat plasma, which comprises the following steps: preparing correction marking working solution with the gradient concentration of the acanthopanax bark glycoside M of 10.0-10000 ng/mL. And diluting the correction marking working solution with each concentration by 20 times by adopting a blank matrix to obtain a correction marking sample, wherein the blank matrix is SD rat plasma without the North acanthopanaxgenin M. Diluting the correction marked sample with 10.0ng/mL of tolbutamide internal standard working solution by 20 times, centrifuging to obtain supernatant, diluting with ultrapure water by 2 times, and adopting LC-MS/MS sample injection analysis to obtain a linear regression equation of the North acanthopanax bark glycoside M. Diluting the SD rat plasma to be tested by 20 times by adopting 10.0ng/mL of tolbutamide internal standard working solution, centrifuging to obtain supernatant, diluting by 2 times by using ultrapure water, adopting LC-MS/MS sample injection analysis, and obtaining the content of the acanthopanax bark glycoside M according to a linear regression equation of the acanthopanax bark glycoside M. The determination method provided by the invention is simple and convenient for sample analysis, and has the advantages of low detection limit, high sensitivity, good repeatability and recovery rate.
Description
Technical Field
The invention relates to the technical field of biological medicine, in particular to a method for measuring the content of acanthopanax bark glycoside M in SD rat plasma.
Background
The northern acanthopanax bark glycoside M has wide application in the processes of scientific research, identification, pharmacological experiment and the like, and has important significance for promoting the development of the technical field of medicine research and development.
The method for measuring the North-acanthopanacis glycoside M in the blood plasma of SD rats is of great significance for researching the metabolism condition of the North-acanthopanacis glycoside M in the blood plasma after administration.
In the prior art, the method for measuring the North acanthopanax bark glycoside M in the SD rat plasma has low test accuracy and poor stability, and brings great inconvenience to research.
Therefore, there is a need for an improvement in the prior art method for determining northern acanthopanaxgenin M in SD rat plasma.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a method for measuring the content of the North acanthopanax bark glycoside M in SD rat plasma, which is simple and convenient for sample analysis, and has low detection limit, high sensitivity and good repeatability and recovery rate.
The invention discloses a method for measuring the content of northern acanthopanax bark glycoside M in SD rat plasma, which is characterized by comprising the following steps:
preparing correction marking working solution with the gradient concentration of the acanthopanax bark glycoside M of 10.0-10000 ng/mL by taking the acanthopanax bark glycoside M as a solute and taking a 50wt% acetonitrile aqueous solution as a solvent;
diluting correction marking working solution of each concentration by 20 times by adopting a blank matrix to obtain a correction marking sample, wherein the blank matrix is SD rat plasma without the North acanthopanaxgenin M;
diluting the correction marked sample with the concentration of 10.0ng/mL of tolbutamide internal standard working solution by 20 times, centrifuging to obtain supernatant, diluting the supernatant with ultrapure water by 2 times, and adopting LC-MS/MS sample injection analysis to obtain a linear regression equation of the North acanthopanax bark glycoside M;
diluting the plasma of the SD rat to be tested by 20 times by adopting 10.0ng/mL of tolbutamide internal standard working solution, centrifuging to obtain supernatant, diluting the supernatant by 2 times by using ultrapure water, adopting LC-MS/MS sample injection analysis, and obtaining the content of the acanthopanacis in the plasma of the SD rat according to a linear regression equation of the acanthopanacis.
Preferably, the LC-MS/MS analysis liquid chromatography conditions include:
stationary phase: an ACE 5C18 chromatographic column with a filler particle diameter of 5 mu m, a diameter of 2.1mm and a length of 50 mm;
mobile phase: a mixed system with mobile phases A and B;
a is ammonium formate and ammonium acetate aqueous solution, the volume ratio of formic acid to ammonium acetate aqueous solution to water is 0.1:0.2:100, and the concentration of ammonium acetate in the ammonium acetate aqueous solution is 1mol/L;
and B is an ammonium formate-ammonium acetate methanol-acetonitrile solution, the volume ratio of formic acid to an ammonium acetate aqueous solution to methanol to acetonitrile is 0.1:0.1:50:50, and the concentration of ammonium acetate in the ammonium acetate aqueous solution is 1mol/L.
Further preferably, the LC-MS/MS analysis liquid chromatography conditions include: flow rate: 0.40mL/min;
column temperature: 40 ℃;
autoinjector temperature: 4 ℃;
sample injection amount: 10 mu L.
Further preferably, the gradient elution procedure in the LC-MS/MS analysis is:
0.01min, 40% by volume of A and 60% by volume of B;
0.90min, wherein the volume percentage of A is 0%, and the volume percentage of B is 100%;
1.60min, wherein the volume percentage of A is 0 percent, and the volume percentage of B is 100 percent;
1.61min, wherein the volume percentage of A is 40 percent, and the volume percentage of B is 60 percent;
2.50min, the volume percentage of A is 40%, and the volume percentage of B is 60%.
Preferably, in LC-MS/MS analysis, the liquid chromatography injector wash is: the weak washing adopts 50% methanol aqueous solution, and the strong washing adopts methanol, acetonitrile, isopropanol and water which are mixed according to the volume ratio of 1:1:1:1.
Preferably, the mass spectrometry conditions in the LC-MS/MS analysis include:
ion source: an electrospray ion source;
ionization mode: a positive ion mode;
the resolution mode is Unit;
the collision gas, the gas curtain gas, the atomization gas, the auxiliary gas 1 and the auxiliary gas 2 are all high-purity nitrogen;
spray voltage 5500V.
The beneficial effects of the invention are as follows:
the method for measuring the content of the North acanthopanax bark glycoside M in the SD rat plasma is simple and convenient for sample analysis, and has the advantages of low detection limit, high sensitivity, good repeatability and recovery rate.
The foregoing and other objects, features and advantages of the invention will be apparent from the following more particular description of preferred embodiments, as illustrated in the accompanying drawings.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a spectrum of the analyte being North-acanthopanax bark glycoside M in a solvent sample in an embodiment of the present invention;
FIG. 2 is a graph of the analyte in a solvent sample of an embodiment of the present invention, tolbutamide;
FIG. 3 is a graph of the analyte being North-acanthopanax bark glycoside M in a double blank sample in an embodiment of the present invention;
FIG. 4 is a graph of the analyte tolbutamide in a double blank sample in an embodiment of the invention;
FIG. 5 is a graph showing the residual effect of the analyte being North acanthopanacis M in an embodiment of the present invention;
FIG. 6 is a graph showing the residual effect of tolbutamide as the analyte in an embodiment of the present invention;
FIG. 7 is a graph of the lower limit of quantification for a calibration marker sample for the analyte being North acanthopanacis M in an embodiment of the present invention;
FIG. 8 is a graph of the lower limit of the quantification of the calibration label for tolbutamide in an embodiment of the present invention;
FIG. 9 is a graph of the upper limit of quantification for a calibration marker sample for the analyte being North acanthopanacis M in an embodiment of the present invention;
FIG. 10 is a graph of the upper limit of the quantification of the calibration marker sample in the present invention for the analyte tolbutamide.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The instruments and reagents used in this example were as follows:
instrument:
high performance liquid chromatography Shimadzu LC-30AD
Mass spectrometer AB SCIEX-5000Q TRAP-LC/MS/MS system
Data acquisition and management analysis 1.6.3,Applied Biosystem
Daily computing/reporting Office 2016or other version,Microsoft
Reagent:
the hollow white matrix in this example was SD rat plasma without containing asiaticoside M collected from the company limited by bio-pharmaceutical in the collar (su zhou), and heparin sodium was used as an anticoagulant.
In this example, the internal standard working solution, 10.0ng/mL of tolbutamide, was mixed with 100wt% acetonitrile, and the concentration of tolbutamide was 10.0ng/mL.
The method for determining the content of the acanthopanax bark glycoside M in the plasma of the SD rat by using the HPLC-MS-MS method comprises the following steps:
1. establishing a linear regression equation of the North acanthopanacis glycoside M
Dissolving the standard substance of the northern acanthopanacis glycoside M in a dimethyl sulfoxide solution to obtain 1.00mg/mL of northern acanthopanacis glycoside M stock solution.
Taking a stock solution of the acanthopanax bark glycoside M, and diluting the stock solution of the acanthopanax bark glycoside M with a 50wt% acetonitrile aqueous solution to obtain a correction marking working solution with the concentration of the acanthopanax bark glycoside M series of 10, 20, 100, 800, 2000, 8000 and 10000 ng/mL.
And respectively taking 10 mu L of correction marking working solution with each concentration and mixing with 190 mu L of blank matrix to respectively obtain correction marking samples with the M series of the North acanthopanax bark glycosides of which the concentrations are 0.5, 1, 5, 40, 100, 400 and 500ng/mL.
Diluting the correction marked sample with each concentration by 20 times by adopting an internal standard working solution, centrifuging to obtain supernatant, diluting the supernatant by 2 times by using ultrapure water, and adopting LC-MS/MS sample injection analysis to obtain a linear regression equation of the North acanthopanax bark glycoside M.
2. Performing methodological test verification on the established linear regression equation of the acanthopanacis glycoside M
1. Quality control sample:
dissolving the standard substance of the northern acanthopanacis glycoside M in a dimethyl sulfoxide solution to obtain 1.00mg/mL of northern acanthopanacis glycoside M stock solution.
And diluting the stock solution of the acanthopanax bark glycoside M with 50wt% acetonitrile water solution to obtain quality control working solutions with the concentration of the acanthopanax bark glycoside M series of 10ng/mL, 30ng/mL, 300ng/mL and high concentration of 7500 ng/mL.
And respectively taking 10 mu L of quality control working solution with each concentration and mixing with 190 mu L of blank matrix to respectively obtain quality control samples of which the concentration of the North acanthopanacis glycoside M series is 0.5ng/mL, the concentration of the North acanthopanacis glycoside M series is 1.5ng/mL, the concentration of the North acanthopanacis glycoside M series is low (QC 3), the concentration of the North acanthopanacis glycoside M series is 15ng/mL, and the concentration of the North acanthopanacis glycoside M series is high (QC 1) 375 ng/mL.
And respectively taking 20 mu L of quality control samples with each concentration, adding 180 mu L of internal standard working solution into the quality control samples with each concentration, uniformly mixing, centrifuging to obtain 50 mu L of supernatant, adding 50 mu L of ultrapure water, uniformly mixing at a low speed by vortex, and adopting LC-MS/MS sample injection analysis.
2. Double blank samples:
double blank samples are blank substrates.
Mixing 20 μl of blank matrix and 180 μl of acetonitrile uniformly, centrifuging to obtain 50 μl of supernatant, adding 50 μl of ultra-pure water, mixing at low speed, and performing sample injection analysis by LC-MS/MS. Wherein acetonitrile is 100wt% acetonitrile. The test results are shown in fig. 3 and fig. 4.
3. Solvent sample:
the solvent sample is ultrapure water.
Mixing 20 μl of ultrapure water and 180 μl of acetonitrile uniformly, centrifuging to obtain 50 μl of supernatant, adding 50 μl of ultrapure water, mixing at low speed by vortex, and analyzing by LC-MS/MS sample injection. Wherein acetonitrile is 100wt% acetonitrile. The test results are shown in fig. 1 and fig. 2.
4. Recovery and matrix effect pure solution, i.e. the coat solution.
The method comprises the steps of mixing a quality control working solution of the northern acanthopanacis, a toluene sulfobutylurea solution and a 50wt% acetonitrile aqueous solution to prepare two parts of heat solution, wherein the concentrations of the northern acanthopanacis and the toluene sulfobutylurea in one part of heat solution are respectively 0.375ng/mL and 22.5ng/mL. In the other part of the coat solution, the concentrations of the North-acanthopanaxgenin M and the tolbutamide are 93.8ng/mL and 22.5ng/mL respectively.
Mixing 20 μl of matrix effect sample and 180 μl of acetonitrile uniformly, centrifuging to obtain 50 μl of supernatant, mixing with 20 μl of heat solution and 30 μl of ultra-pure water by low-speed vortex, and analyzing by LC-MS/MS sample injection. The matrix effect samples were at least 6 batches of blank matrix. Wherein acetonitrile is 100wt% acetonitrile. For both concentration levels of the coat solution, an investigation was performed.
Mixing 20 μl of recovery rate sample, namely blank matrix, 180 μl of acetonitrile, centrifuging to obtain 50 μl of supernatant, mixing with 20 μl of heat solution and 30 μl of water solution at low speed by vortex, and analyzing by LC-MS/MS sample injection. Wherein acetonitrile is 100wt% acetonitrile. For both concentration levels of the coat solution, an investigation was performed.
Mixing 20 μl of pure liquid sample, i.e. ultrapure water and 180 μl of acetonitrile uniformly, centrifuging to obtain 50 μl of supernatant, mixing with 20 μl of heat solution and 30 μl of water solution by low-speed vortex uniformly, and analyzing by LC-MS/MS sample injection. Wherein acetonitrile is 100wt% acetonitrile. For both concentration levels of the coat solution, an investigation was performed.
The test results are shown in fig. 7 and 8.
5. Calibration marking sample
Calibration marker samples were taken with a concentration of P.North-containing M of 0.5ng/mL (lower limit of quantitation) and 500ng/mL (upper limit of quantitation).
And respectively taking 20 mu L of each concentration correction marking sample, adding 180 mu L of internal standard working solution into each concentration correction marking sample, uniformly mixing, centrifuging to obtain 50 mu L of supernatant, adding 50 mu L of ultrapure water, uniformly mixing at a low speed by vortex, and adopting LC-MS/MS sample injection analysis. The test results are shown in fig. 9 and 10.
3. Analysis of linear regression equation methodology validation test of North-acanthopanaxoside M
And judging the accuracy of a linear regression equation of the northern acanthopanacis glycoside M according to the result of the methodological verification test, and if the accuracy meets the standard, determining the northern acanthopanacis glycoside M in SD rat blood plasma.
4. Determination of North acanthopanacis glycoside M in SD rat plasma to be tested
Diluting the plasma of the SD rat to be tested by 20 times by adopting 10.0ng/mL of tolbutamide internal standard working solution, centrifuging to obtain supernatant, diluting the supernatant by 2 times by using ultrapure water, adopting LC-MS/MS sample injection analysis, and obtaining the content of the acanthopanax bark glycoside M in the plasma of the SD rat according to a linear regression equation of the acanthopanax bark glycoside M.
In the LC-MS/MS analysis and detection step described above in this embodiment, the liquid chromatography conditions are:
stationary phase: an ACE 5C18 chromatographic column with a filler particle diameter of 5 mu m, a diameter of 2.1mm and a length of 50 mm;
mobile phase: the mobile phase is a mixed system of A and B, A is an ammonium formate and acetic acid aqueous solution, wherein formic acid: ammonium acetate (1M): the volume ratio of water is 0.1:0.2:100; b is ammonium formate, acetic acid, methanol and acetonitrile solution, wherein formic acid: ammonium acetate (1M): methanol: acetonitrile in a volume ratio of 0.1:0.1:50:50;
the elution gradient is:
0.01min, 40% by volume of A and 60% by volume of B;
0.90min, wherein the volume percentage of A is 0%, and the volume percentage of B is 100%;
1.60min, wherein the volume percentage of A is 0 percent, and the volume percentage of B is 100 percent;
1.61min, wherein the volume percentage of A is 40 percent, and the volume percentage of B is 60 percent;
2.50min, the volume percentage of A is 40%, and the volume percentage of B is 60%.
The sample injector cleaning liquid is as follows: weak wash is sample injector washing liquid 1, sample injector washing liquid 1 is 50% methanol water solution, and the preparation method of 50% methanol water solution comprises adding 500mL acetonitrile and 500mL H into 1L glass bottle 2 And O, uniformly mixing.
The strong washing is a sample injector washing liquid 2, and the sample injector washing liquid 2 is formed by mixing methanol, acetonitrile, isopropanol and water according to a volume ratio of 1:1:1:1. The preparation method of the injector cleaning liquid 2 is to add 250mL of methanol, 250mL of acetonitrile, 250mL of isopropanol and 250mL of water into a 1L glass bottle, and mix the materials uniformly.
Flow rate: 0.40mL/min;
column temperature: 40 ℃;
autoinjector temperature: 4 ℃;
sample injection amount: 10 mu L.
The retention time of the northern acanthopanacis glycoside M was about 1.33min and the retention time of the tolbutamide was about 0.75min at the time of injection.
In the detection step, detection is carried out according to the following mass spectrum conditions:
ion source: an electrospray ion source;
ionization mode: a positive ion mode;
the resolution mode is Unit;
the collision gas, the gas curtain gas, the atomization gas, the auxiliary gas 1 and the auxiliary gas 2 are all high-purity nitrogen;
spray voltage 5500V.
The regression and data processing method of the embodiment is as follows:
regression model y=ax+b, linear regression, weight factor 1/x 2 Y is the peak area ratio of analyte to internal standard and x is the concentration of analyte in the calibration label.
The calculation software was analytical 1.6.3 and Microsoft Office 2016 (or other version), with all concentration values retaining the 3 significant digits and the% Bias and% CV to the 1-bit after the decimal point.
Analyte: north acanthopanacis glycoside M;
a substrate: SD rat plasma (heparin sodium as anticoagulant);
correction curve range: 0.5 ng/mL-500 ng/mL;
lower limit of quantification: 0.5ng/mL;
linear range: 0.5 ng/mL-500 ng/mL.
The principles and embodiments of the present invention have been described in detail with reference to specific examples, which are provided to facilitate understanding of the method and core ideas of the present invention; meanwhile, as those skilled in the art will have variations in the specific embodiments and application scope in accordance with the ideas of the present invention, the present description should not be construed as limiting the present invention in view of the above.
Claims (3)
1. The method for determining the content of the acanthopanax bark glycoside M in the plasma of the SD rat is characterized by comprising the following steps of:
preparing correction marking working solution with the gradient concentration of the acanthopanax bark glycoside M of 10.0-10000 ng/mL by taking the acanthopanax bark glycoside M as a solute and taking a 50wt% acetonitrile aqueous solution as a solvent;
diluting correction marking working solution of each concentration by 20 times by adopting a blank matrix to obtain a correction marking sample, wherein the blank matrix is SD rat plasma without the North acanthopanaxgenin M;
diluting correction marking samples with 10.0ng/mL of tolbutamide internal standard working solution by 20 times, taking acetonitrile as a solvent in the internal standard working solution, centrifuging to obtain supernatant, diluting the supernatant by 2 times with ultrapure water, and adopting LC-MS/MS sample injection analysis to obtain a linear regression equation of the North acanthopanax bark glycoside M;
diluting the plasma of an SD rat to be detected by 20 times by adopting 10.0ng/mL of tolbutamide internal standard working solution, centrifuging to obtain supernatant, diluting the supernatant by 2 times by using ultrapure water, adopting LC-MS/MS sample injection analysis, and obtaining the content of the acanthopanacis in the plasma of the SD rat according to a linear regression equation of the acanthopanacis;
the liquid chromatography conditions in the LC-MS/MS analysis include: flow rate: 0.40mL/min;
column temperature: 40 ℃;
autoinjector temperature: 4 ℃;
sample injection amount: 10. Mu.L;
stationary phase: an ACE 5C18 chromatographic column with a filler particle size of 5 mu m, a diameter of 2.1mm and a length of 50 mm;
mobile phase: a mixed system with mobile phases A and B;
a is ammonium formate and ammonium acetate aqueous solution, the volume ratio of formic acid to ammonium acetate aqueous solution to water is 0.1:0.2:100, and the concentration of ammonium acetate in the ammonium acetate aqueous solution is 1mol/L;
b is ammonium formate and acetic acid methanol acetonitrile solution, the volume ratio of formic acid to ammonium acetate aqueous solution to methanol to acetonitrile is 0.1:0.1:50:50, and the concentration of ammonium acetate in the ammonium acetate aqueous solution is 1mol/L;
the gradient elution procedure in the LC-MS/MS analysis is:
0.01min, 40% by volume of A and 60% by volume of B;
0.90min, wherein the volume percentage of A is 0%, and the volume percentage of B is 100%;
1.60min, wherein the volume percentage of A is 0 percent, and the volume percentage of B is 100 percent;
1.61min, wherein the volume percentage of A is 40 percent, and the volume percentage of B is 60 percent;
2.50min, the volume percentage of A is 40%, and the volume percentage of B is 60%.
2. The method for determining the content of the northern acanthopanacis glucoside M in the plasma of the SD rat according to claim 1, wherein in the LC-MS/MS analysis, the liquid chromatographic injector cleaning liquid is: the weak washing adopts 50% methanol aqueous solution, and the strong washing adopts methanol, acetonitrile, isopropanol and water which are mixed according to the volume ratio of 1:1:1:1.
3. The method for determining the content of northern acanthopanacis glucoside M in SD rat plasma according to claim 1, wherein the mass spectrometry conditions in the LC-MS/MS analysis include:
ion source: an electrospray ion source;
ionization mode: a positive ion mode;
the resolution mode is Unit;
the collision gas, the gas curtain gas, the atomization gas, the auxiliary gas 1 and the auxiliary gas 2 are all high-purity nitrogen;
spray voltage 5500V.
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| CN106153792A (en) * | 2015-03-23 | 2016-11-23 | 天士力制药集团股份有限公司 | The finger printing of a kind of Cortex Periplocae and quality determining method thereof |
| CN109776299A (en) * | 2017-11-13 | 2019-05-21 | 青岛凯玉盈商贸有限公司 | A kind of extraction separation method of cortex periplocae chemical component |
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