CN114720580A - Method for detecting sitagliptin and metformin in biological sample - Google Patents
Method for detecting sitagliptin and metformin in biological sample Download PDFInfo
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- CN114720580A CN114720580A CN202210069300.XA CN202210069300A CN114720580A CN 114720580 A CN114720580 A CN 114720580A CN 202210069300 A CN202210069300 A CN 202210069300A CN 114720580 A CN114720580 A CN 114720580A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention provides a method for detecting sitagliptin and metformin in a biological sample, which adopts an LC-MS/MS method for detection, and has the following chromatographic conditions: a chromatographic column: ZORBAX SB-C184.6 x 150mm,3.5 μm column; mass spectrum conditions: API 4000(ESI source) mass spectrum, positive ion, ion spray voltage 5500V, temperature 550 ℃, atomization gas pressure 55psi, de-clustering voltage pressure 55psi, gas curtain gas pressure 20psi, scanning mode for Multiple Reaction Monitoring (MRM). Mobile phase: a-0.1% aqueous formic acid (containing 5mM ammonium acetate), B-acetonitrile; flow rate: 1.00 ml/min; column temperature: 40 ℃; sample introduction amount: 3.00. mu.l. The method disclosed by the invention can be used for specially, sensitively and quickly measuring the concentrations of sitagliptin and metformin in human plasma, and is mainly suitable for measuring the contents of sitagliptin and metformin in tablets.
Description
Technical Field
The invention belongs to the field of drug chromatography and mass spectrometry, relates to a detection method of chemicals, and particularly relates to a detection method of sitagliptin and metformin in a biological sample.
Background
Sitagliptin belongs to a potent and highly selective dipeptidyl peptidase-4 (DPP-4) inhibitor, metformin is a biguanide oral hypoglycemic drug, and sitagliptin metformin tablets are hypoglycemic drugs with two complementary action mechanisms The compound preparation is matched with diet and exercise therapy and is used for treating type 2 diabetes patients with poor blood sugar control or undergoing combined treatment of the metformin and the drug. The drug was originally developed by Ministry of Mersando, approved by FDA in 2007, and approved in China in 2012 under the name of Meishadong
Currently, there is no method for simultaneously detecting the two components sitagliptin and metformin, and a technical gap is generated in this respect.
Disclosure of Invention
The technical problem to be solved is as follows: aiming at the blank of the existing detection method for simultaneously detecting sitagliptin and metformin, the invention provides the detection method for detecting the sitagliptin and the metformin, which has the advantages of simple operation and quick analysis, and can be applied to various different biological matrixes.
The technical scheme is as follows: a method for detecting sitagliptin and metformin in a biological sample comprises the following steps:
(1) preparing standard yeast working solution: accurately weighing 10.09mg (the mass correction coefficient is 99.1%) of sitagliptin, placing the sitagliptin into a 15mL plastic tube, and dissolving 1mg/mL of sitagliptin by using dimethyl sulfoxide to obtain a sitagliptin stock solution; precisely weighing 10.22mg of metformin hydrochloride (the mass correction coefficient is 77.9%), placing the metformin hydrochloride into a 15mL plastic tube, and dissolving 1mg/mL of metformin hydrochloride by using methanol to obtain a metformin stock solution; diluting the sitagliptin stock solution and the metformin stock solution by 50% methanol water to prepare a mixed standard yeast working solution, wherein the concentration range of the metformin working solution is 160-80000 ng/mL, and the concentration range of the sitagliptin working solution is 20.0-10000 ng/mL;
(2) Preparing a quality control working solution: 10.35mg of sitagliptin (the mass correction coefficient is 99.1%) is placed in a 15mL plastic tube, and 1mg/mL of sitagliptin is dissolved by dimethyl sulfoxide to be used as a sitagliptin stock solution; precisely weighing 10.19mg (mass correction coefficient is 77.9%) of metformin hydrochloride, placing the metformin hydrochloride into a 15mL plastic tube, and dissolving 1mg/mL of metformin hydrochloride by using methanol to obtain a metformin stock solution; diluting the sitagliptin stock solution and the metformin stock solution by 50% methanol water to prepare a mixed quality control working solution, wherein the concentration of the metformin quality control working solution is 480, 12800 and 64000ng/mL, and the concentration of the sitagliptin quality control working solution is 60.0, 1600 and 8000 ng/mL;
(3) preparing an internal standard working solution: taking sitagliptin-d 41mg, placing the sitagliptin-d 41mg in a 1.5mL plastic tube, and dissolving 1mg/mL by using dimethyl sulfoxide to obtain a sitagliptin-d 4 stock solution; taking metformin hydrochloride-d 61mg, placing in a 1.5mL plastic tube, dissolving 1mg/mL with methanol to obtain metformin-d 6 stock solution; diluting the sitagliptin-d 4 stock solution and the metformin-d 6 stock solution with acetonitrile to prepare a mixed internal standard working solution, wherein the concentration of the metformin-d 6 is 20.0ng/mL, and the concentration of the sitagliptin-d 4 is 20.0 ng/mL;
(4) pretreatment of a biological sample: pretreatment of standard yeast quality control: taking a blank biological sample 190 mu L to a 1.5mLEP tube, respectively and uniformly mixing with 10 mu L of standard curve working solution and quality control working solution, then respectively taking 100 mu L of uniformly mixed sample, adding 500 mu L of internal standard working solution (adding 500 mu L of acetonitrile into a double blank sample), whirling for 1min, 15400 +/-10 g, centrifuging for 10min at 4 ℃, and taking 100 mu L of supernatant for sample injection analysis; taking 100 mu L of biological sample, adding 500 mu L of internal standard working solution, whirling for 1min, centrifuging for 10min at 15400 +/-10 g and 4 ℃, and taking 100 mu L of supernatant for sample injection analysis;
(5) LC-MS/MS method detection
And (3) detecting by an LC-MS/MS method, and obtaining a standard curve by a normalization method based on the peak area ratio of the substance to be detected and the internal standard, so as to quantitatively obtain the concentrations of sitagliptin and metformin in the biological sample.
Preferably, the chromatographic and mass spectrum conditions of the LC-MS/MS method are as follows:
chromatographic conditions are as follows:
a chromatographic column: ZORBAX SB-C184.6 x 150mm,3.5 μm, Agilent;
mobile phase: 0.1% aqueous formic acid (containing 5mM ammonium acetate), B-acetonitrile;
flow rate: 1.00 ml/min;
column temperature: 40 ℃;
sample introduction amount: 3.00 mu l;
isocratic program: mobile phase ratio: a, B and 30:70
Mass spectrum conditions:
electrospray positive ion mode;
spraying voltage: 5500V;
air curtain gas (CUR): 20 psi;
collision induced pyrolysis (CAD): 10;
atomizing gas (GS 1): 55psi
Assist gas (GS 2): 55psi
The scanning mode is as follows: multiple Reaction Monitoring (MRM).
Preferably, the biological sample in step (4) is selected from a plasma sample of the subject.
Preferably, the multiple reaction monitoring parameters are:
has the advantages that:
the invention provides a biological sample analysis method for simultaneously determining sitagliptin and metformin, which is used for carrying out combined analysis on the sitagliptin and the metformin by a high-efficiency, quick and sensitive liquid phase-mass spectrum combined system (LC-MS) method. The method adopts a simple organic solvent protein precipitation method to carry out pretreatment on the biological sample, and obtains a standard curve through a normalization method based on the peak area ratio of the substance to be detected and the internal standard, thereby quantitatively obtaining the concentrations of sitagliptin and metformin in the biological sample. The method provides a simple and convenient analysis method for detecting sitagliptin and metformin in the pharmacokinetics of the sitagliptin and the metformin in a human body. The detection method is simple to operate and rapid in analysis, and can be applied to various different biological matrixes.
Description of the drawings:
FIG. 1 is a chromatogram of metformin and an internal standard, wherein FIG. 1(A) is the metformin chromatogram and FIG. 1(B) is the internal standard chromatogram.
Fig. 2 is a chromatogram of sitagliptin and an internal standard, wherein fig. 2(a) is the sitagliptin chromatogram, and fig. 2(B) is the internal standard chromatogram.
FIG. 3 is a standard curve of metformin based on peak area ratio of the analyte to the internal standard by normalization.
FIG. 4 is a standard curve obtained by a normalization method based on the peak area ratio of the substance to be detected to the internal standard.
Fig. 5 is a chromatogram for detecting sitagliptin and an internal standard in a plasma sample of a subject, wherein fig. 5(a) is a sitagliptin chromatogram, and fig. 5(B) is an internal standard chromatogram.
FIG. 6 is a chromatogram for detecting metformin and an internal standard in a plasma sample from a subject, wherein FIG. 6(A) is a metformin chromatogram and FIG. 6(B) is an internal standard chromatogram.
Detailed Description
Instruments and reagents: instruments and reagents: high performance liquid chromatograph: SHIMADZU HPLC; a chromatographic column: ZORBAX SB-C184.6 x 150mm,3.5 μm, Agilent; sitagliptin standard (MACKCIN); metformin hydrochloride standard (national institute of food and drug testing); sitagliptin-d 4(TLC Pharmaceutical Standards) and metformin hydrochloride-d 6 standard (Toronto Fisher Scientific); formic acid, ammonium acetate and acetonitrile were purchased from Thermo Fisher Scientific.
Example 1
A method for detecting sitagliptin and metformin in a biological sample comprises the following steps:
(1) chromatographic conditions are as follows:
a chromatographic column: ZORBAX SB-C184.6 x 150mm,3.5 μm, Agilent;
mobile phase: 0.1% aqueous formic acid (containing 5mM ammonium acetate), B-acetonitrile;
flow rate: 1.00 ml/min;
column temperature: 40 ℃;
sample introduction amount: 3.00 mu l;
isocratic program: mobile phase ratio: a, B and 30:70
Mass spectrum conditions:
electrospray positive ion mode;
spraying voltage: 5500V;
air curtain gas (CUR): 20 psi;
collision induced pyrolysis (CAD): 10;
atomizing gas (GS 1): 55psi
Assist gas (GS 2): 55psi
The scanning mode is as follows: multiple Reaction Monitoring (MRM):
(2) preparing standard yeast working solution: accurately weighing 10.09mg (the mass correction coefficient is 99.1%) of sitagliptin, placing the sitagliptin into a 15mL plastic tube, and dissolving 1mg/mL of sitagliptin by using dimethyl sulfoxide to obtain a sitagliptin stock solution; precisely weighing 10.22mg of metformin hydrochloride (the mass correction coefficient is 77.9%), placing the metformin hydrochloride into a 15mL plastic tube, and dissolving 1mg/mL of metformin hydrochloride by using methanol to obtain a metformin stock solution; diluting the sitagliptin stock solution and the metformin stock solution by 50% methanol water to prepare a mixed standard yeast working solution, wherein the concentration range of the metformin working solution is 160-80000 ng/mL, and the concentration range of the sitagliptin working solution is 20.0-10000 ng/mL;
(3) Preparing a quality control working solution: 10.35mg of sitagliptin (with a mass correction coefficient of 99.1%) is placed in a 15mL plastic tube, and 1mg/mL of sitagliptin is dissolved by dimethyl sulfoxide to serve as a sitagliptin stock solution; precisely weighing 10.19mg (mass correction coefficient is 77.9%) of metformin hydrochloride, placing the metformin hydrochloride into a 15mL plastic tube, and dissolving 1mg/mL of metformin hydrochloride by using methanol to obtain a metformin stock solution; diluting the sitagliptin stock solution and the metformin stock solution by 50% methanol water to prepare a mixed quality control working solution, wherein the concentration of the metformin quality control working solution is 480, 12800 and 64000ng/mL, and the concentration of the sitagliptin quality control working solution is 60.0, 1600 and 8000 ng/mL; (4) preparing an internal standard working solution: placing a sitagliptin-d 41mg in a 1.5mL plastic tube, and dissolving 1mg/mL by using dimethyl sulfoxide to obtain a sitagliptin-d 4 stock solution; taking metformin hydrochloride-d 61mg, placing in a 1.5mL plastic tube, dissolving 1mg/mL with methanol to obtain metformin-d 6 stock solution; diluting the sitagliptin-d 4 stock solution and the metformin-d 6 stock solution with acetonitrile to prepare a mixed internal standard working solution, wherein the concentration of the metformin-d 6 is 20.0ng/mL, and the concentration of the sitagliptin-d 4 is 20.0 ng/mL;
(5) pretreatment of a biological sample: pretreatment of standard yeast quality control: taking blank biological samples 190 mu L to 1.5mLEP tubes, respectively and uniformly mixing with 10 mu L of standard curve working solution and quality control working solution, then respectively taking 100 mu L of uniformly mixed samples, adding 500 mu L of internal standard working solution (adding 500 mu L of acetonitrile into double blank samples), carrying out vortex 1min, 15400 +/-10 g, centrifuging for 10min at 4 ℃, and taking 100 mu L of supernatant for sample injection analysis; taking 100 mu L of plasma sample of a subject, adding 500 mu L of internal standard working solution, vortexing for 1min, 15400 +/-10 g, centrifuging for 10min at 4 ℃, and taking 100 mu L of supernatant for sample injection analysis;
(6) LC-MS/MS method detection
And (3) detecting by the LC-MS/MS method, and obtaining a standard curve by a normalization method based on the peak area ratio of the object to be detected and the internal standard, so as to quantitatively obtain the concentrations of sitagliptin and metformin in the biological sample.
(7) Chromatogram acquisition
And (3) performing sample injection analysis to obtain chromatograms of sitagliptin and the internal standard, wherein the chromatograms are shown in figure 1. Wherein FIG. 1(A) is a sitagliptin chromatogram, and FIG. 1(B) is an internal standard chromatogram. The chromatograms of metformin and internal standard are shown in FIG. 2. Wherein FIG. 2(A) is a sitagliptin chromatogram, and FIG. 2(B) is an internal standard chromatogram.
(8) Standard curve
Based on the peak area ratio of the substance to be detected and the internal standard, the sitagliptin obtains a standard curve by a normalization method, and as shown in fig. 3, the standard equation is as follows: y 0.00721x +0.000295(r 0.9997). The metformin is based on the peak area ratio of the substance to be detected and the internal standard, and a standard curve is obtained by a normalization method, as shown in fig. 4, the standard equation is as follows: y 0.00232x +0.00168(r 0.9995).
(9) Quantitative results
The concentrations of sitagliptin and metformin quantitatively obtained from human plasma biological samples by a standard curve are shown in table 1:
TABLE 1
| Time point (h) | Sitagliptin concentration (ng/mL) | Dimehypo (dimethyl) Guanidine concentration (ng/mL) |
| 0 | 0.00 | 0.00 |
| 0.5 | 11.0 | 1270 |
| 1 | 44.8 | 3770 |
| 1.5 | 90.4 | 3480 |
| 2 | 158 | 2770 |
| 2.33 | 218 | 2660 |
| 2.67 | 208 | 2560 |
| 3 | 201 | 2420 |
| 3.5 | 233 | 2380 |
| 4 | 215 | 2120 |
| 5 | 237 | 1980 |
| 6 | 209 | 1770 |
| 8 | 182 | 1310 |
| 10 | 163 | 1090 |
| 12 | 132 | 761 |
| 15 | 92.0 | 471 |
| 24 | 37.5 | 93.1 |
| 36 | 16.1 | 23.0 |
| 48 | 8.84 | 16.6 |
Although the present invention has been described in detail in the examples by way of general illustration, specific embodiments and experiments, it is to be understood that modifications and improvements may be made without departing from the spirit of the invention and within the scope of the following claims.
Claims (4)
1. A method for detecting sitagliptin and metformin in a biological sample is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing standard yeast working solution: accurately weighing 10.09mg of sitagliptin, placing the sitagliptin in a 15mL plastic tube, and dissolving 1mg/mL of sitagliptin by using dimethyl sulfoxide to obtain a sitagliptin stock solution; precisely weighing 10.22mg of metformin hydrochloride, placing the metformin hydrochloride into a 15mL plastic tube, and dissolving 1mg/mL of metformin hydrochloride by using methanol to obtain a metformin stock solution; diluting the sitagliptin stock solution and the metformin stock solution by 50% methanol water to prepare a mixed standard yeast working solution, wherein the concentration range of the metformin working solution is 160-80000 ng/mL, and the concentration range of the sitagliptin working solution is 20.0-10000 ng/mL;
(2) preparing a quality control working solution: 10.35mg of sitagliptin, placing the sitagliptin in a 15mL plastic tube, and dissolving 1mg/mL of sitagliptin by using dimethyl sulfoxide to obtain a sitagliptin stock solution; precisely weighing 10.19mg of metformin hydrochloride, placing the metformin hydrochloride into a 15mL plastic tube, and dissolving 1mg/mL of metformin hydrochloride by using methanol to obtain a metformin stock solution; diluting the sitagliptin stock solution and the metformin stock solution by 50% methanol water to prepare a mixed quality control working solution, wherein the concentration of the metformin quality control working solution is 480, 12800 and 64000ng/mL, and the concentration of the sitagliptin quality control working solution is 60.0, 1600 and 8000 ng/mL;
(3) Preparing an internal standard working solution: placing a sitagliptin-d 41mg in a 1.5mL plastic tube, and dissolving 1mg/mL by using dimethyl sulfoxide to obtain a sitagliptin-d 4 stock solution; taking metformin hydrochloride-d 61mg, placing in a 1.5mL plastic tube, dissolving 1mg/mL with methanol to obtain metformin-d 6 stock solution; diluting the sitagliptin-d 4 stock solution and the metformin-d 6 stock solution with acetonitrile to prepare a mixed internal standard working solution, wherein the concentration of the metformin-d 6 is 20.0ng/mL, and the concentration of the sitagliptin-d 4 is 20.0 ng/mL;
(4) pretreatment of a biological sample: pretreatment of standard yeast quality control: taking a blank biological sample 190 mu L to a 1.5mLEP tube, respectively and uniformly mixing with 10 mu L of standard curve working solution and quality control working solution, then respectively taking 100 mu L of the uniformly mixed sample, adding 500 mu L of internal standard working solution, carrying out vortex for 1min, 15400 +/-10 g, centrifuging for 10min at 4 ℃, and taking 100 mu L of supernatant for sample injection analysis; taking 100 mu L of biological sample, adding 500 mu L of internal standard working solution, whirling for 1min, centrifuging for 10min at 15400 +/-10 g and 4 ℃, and taking 100 mu L of supernatant for sample injection analysis;
(5) LC-MS/MS method detection
And (3) detecting by an LC-MS/MS method, and obtaining a standard curve by a normalization method based on the peak area ratio of the substance to be detected and the internal standard, so as to quantitatively obtain the concentrations of sitagliptin and metformin in the biological sample.
2. The method for detecting sitagliptin and metformin according to claim 1, wherein: the chromatographic and mass spectrum conditions of the LC-MS/MS method are as follows:
chromatographic conditions are as follows:
a chromatographic column: ZORBAX SB-C184.6 mm, 3.5 μm;
mobile phase: 0.1% aqueous formic acid containing 5mM ammonium acetate, B-acetonitrile;
flow rate: 1.00 ml/min;
column temperature: 40 ℃;
sample introduction amount: 3.00 mu l;
isocratic program: mobile phase ratio: a, B and 30:70
Mass spectrum conditions:
electrospray positive ion mode;
spraying voltage: 5500V;
air curtain air: 20 psi;
collision-induced pyrolysis: 10;
atomizing: 55psi
Auxiliary gas: 55psi
The scanning mode is as follows: and (5) monitoring multiple reactions.
3. The method for detecting sitagliptin and metformin according to claim 1, wherein: the biological sample in step (4) is selected from a plasma sample of the subject.
4. The method for detecting sitagliptin and metformin according to claim 2, wherein: the multiple reaction monitoring parameters are:
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114397380A (en) * | 2021-12-15 | 2022-04-26 | 安徽万邦医药科技股份有限公司 | Method for determining concentration of western-style gliptin in blood plasma by liquid chromatography-mass spectrometry |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114397380A (en) * | 2021-12-15 | 2022-04-26 | 安徽万邦医药科技股份有限公司 | Method for determining concentration of western-style gliptin in blood plasma by liquid chromatography-mass spectrometry |
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