CN112326842A - Saxagliptin quantitative detection and analysis method - Google Patents
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Abstract
The invention relates to the technical field of detection and analysis, and particularly discloses a method for quantitative detection and analysis of saxagliptin, which specifically comprises the following steps: (1) preparing saxagliptin standard working solutions with 9 concentration gradients, and (2) preparing an internal standard solution with 50 ng/mL; (3) taking a plasma sample, adding an internal standard solution and acetonitrile, and taking a supernatant after vortex and centrifugation; (4) transferring the treated supernatant into a centrifuge tube, drying the centrifuge tube with nitrogen at room temperature, redissolving the residue with 200 mu L of 10% methanol, and taking the supernatant after vortex and centrifugation; (5) after a blank plasma sample is treated and purified, adding a standard working solution with a concentration gradient to obtain a matrix standard working solution of saxagliptin with a series of concentrations; (6) and (6) sample injection detection. The invention overcomes the defects of the prior art, and adopts ultra-high performance liquid chromatography-tandem mass spectrometry to greatly improve the sensitivity of the detection method; the method has good stability and strong universality, and can sensitively and rapidly determine the blood concentration of saxagliptin in plasma.
Description
Technical Field
The invention relates to the technical field of detection and analysis, and particularly belongs to a method for quantitative detection and analysis of saxagliptin.
Background
Saxagliptin (saxagliptin) is used for treating type II diabetes and is marketed by the original manufacturers in 2009 as Behcet. Saxagliptin is a high-efficiency dipeptidyl peptidase4 (DPP-4) inhibitor, and can increase the levels of endogenous Glucagon-like peptide-1 (Glucagon-like peptide-1, GLP-1) and Glucose-dependent insulinotropic peptide (GIP) through selectively inhibiting DPP-4, thereby regulating blood sugar.
GLP-1 is secreted in intestinal tract immediately after meal intake, so as to stimulate pancreas to produce glucose-dependent insulin secretion, inhibit glucagon secretion and delay gastric emptying. Under a physiological state, the DPP-4 can rapidly degrade GLP-1 and GIP to lose activity, and the endogenous GLP-1 level can be increased by 3-4 times by taking the DPP-4 inhibitor, so that glycated hemoglobin (HbA1c) and postprandial blood sugar are effectively reduced, the weight is not influenced, and the risk of hypoglycemia is not obvious. Several clinical studies of saxagliptin were published in succession, and consistently demonstrated their reduced HbA1c, Fasting Plasma Glucose (FPG), postprandial blood glucose (PPG) levels, as well as their good tolerability and safety profile.
At present, documents for detecting specific content of saxagliptin in a biological sample are few, and how to rapidly and stably quantitatively detect saxagliptin is a problem to be solved in the industry.
Disclosure of Invention
The invention aims to provide a method for quantitatively detecting and analyzing saxagliptin, which overcomes the defects of the prior art, is simple in processing method and operation, and can quickly detect the content of the saxagliptin in a biological sample.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a method for quantitative detection and analysis of saxagliptin comprises the following steps:
(1) preparation of standard working solutions: precisely weighing a saxagliptin reference substance, dissolving and diluting the reference substance with 50% acetonitrile, and then diluting the reference substance with 10% methanol to obtain standard working solutions with 9 concentration gradients;
(2) preparation of internal standard solution: precisely weighing a saxagliptin reference substance, dissolving and diluting the reference substance with 50% acetonitrile to prepare an internal standard stock solution with the mass concentration of 1mg/mL, and then diluting the internal standard stock solution with 10% methanol to prepare an internal standard solution with the mass concentration of 50 ng/mL;
(3) plasma sample treatment: taking 100 mu L of plasma sample, putting the plasma sample into a 1.5mL centrifuge tube, respectively adding 50 mu L of 50ng/mL internal standard solution and 500 mu L of acetonitrile, and taking supernate after vortex and centrifugation;
(4) sample purification: transferring the supernatant obtained in the step (3) into a 1.5mL centrifuge tube, drying the centrifuge tube with nitrogen at room temperature, re-dissolving the residue with 200 mu L10% methanol, performing vortex and centrifugation, and then taking the supernatant to obtain a sample of saxagliptin to be detected for ultra performance liquid chromatography tandem mass spectrometry;
(5) matrix standard working solution: treating and purifying the blank plasma sample according to the steps (2) and (3), drying the blank plasma sample by blowing nitrogen, adding 10 mu L of the standard working solution with the gradient concentration prepared in the step (1), and uniformly mixing the standard working solution with the substrate of saxagliptin with the series of concentrations in a vortex manner;
(6) sample introduction detection: and (3) injecting the substrate standard working solution of the saxagliptin with the series of concentrations prepared in the step (4) and the sample injection product of the saxagliptin to be detected prepared in the step (3) into a liquid chromatograph, and detecting by a tandem mass spectrometer to obtain the content of the saxagliptin in the plasma.
Further, the concentration gradient of the standard working solution in the step (1) is 0.1ng/mL, 1.5ng/mL, 10ng/mL, 20ng/mL, 40ng/mL, 50ng/mL, 80ng/mL and 100 ng/mL.
Further, in the step (2) and the step (3), the vortex time is 2min, the vortex rotation speed at room temperature is 4500rpm, the centrifugation time is 10min, and the centrifugation speed is 13500 r/min.
Further, the determination of the liquid chromatography conditions in the step (5) is as follows: a chromatographic column: the chromatographic column is Waters BEH Shield RP18(ii) a Mobile phase: 10mmol/L ammonium acetate-acetonitrile (70: 30, V/V); flow rate: 0.3 mL/min; column temperature: 30 ℃; sample introduction amount: 10.0. mu.L.
Further, the mass spectrum measuring conditions in the step (5) are as follows: an ion source: ESI, positive ion mode; capillary voltage: 4.0 kv; ion source temperature: 110 ℃; the temperature of desolventizing gas is 350 ℃; desolventizing agent gas flow: 800L/hr; the cone hole blowback air flow is 50L/hr; taper hole voltage: 30 v; the scanning mode is as follows: positive ion Multiple Reaction Monitoring (MRM); ion pairing: 316.2/180.2.
Compared with the prior art, the invention has the following implementation effects:
1. the invention establishes a method which has good stability and strong universality and can sensitively and rapidly determine the blood concentration of saxagliptin in plasma.
2. The method has the advantages of simple sample treatment mode, less reagent usage amount for sample extraction and cost saving.
3. The invention adopts ultra-high performance liquid chromatography-tandem mass spectrometry, greatly improves the sensitivity of the detection method, and simultaneously has the advantages of high accuracy, good repeatability and the like.
Drawings
Fig. 1 is an ion scanning mass spectrum of saxagliptin in the method for quantitative detection and analysis of saxagliptin provided by the present invention.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples, and any modification is within the scope of the present invention without departing from the spirit of the present invention.
Example 1
A method for quantitative detection and analysis of saxagliptin comprises the following steps:
(1) preparation of standard working solutions: precisely weighing a saxagliptin reference substance, dissolving and diluting the reference substance with 50% acetonitrile, and then diluting the reference substance with 10% methanol to obtain standard working solutions with 9 concentration gradients;
(2) preparation of internal standard solution: precisely weighing a saxagliptin reference substance, dissolving and diluting the reference substance with 50% acetonitrile to prepare an internal standard stock solution with the mass concentration of 1mg/mL, and then diluting the internal standard stock solution with 10% methanol to prepare an internal standard solution with the mass concentration of 50 ng/mL;
(3) plasma sample treatment: taking 100 mu L of plasma sample, putting the plasma sample into a 1.5mL centrifuge tube, respectively adding 50 mu L of 50ng/mL internal standard solution and 500 mu L of acetonitrile, and taking supernate after vortex and centrifugation;
(4) sample purification: transferring the supernatant obtained in the step (3) into a 1.5mL centrifuge tube, drying the centrifuge tube with nitrogen at room temperature, re-dissolving the residue with 200 mu L10% methanol, performing vortex and centrifugation, and then taking the supernatant to obtain a sample of saxagliptin to be detected for ultra performance liquid chromatography tandem mass spectrometry;
(5) matrix standard working solution: treating and purifying the blank plasma sample according to the steps (2) and (3), drying the blank plasma sample by blowing nitrogen, adding 10 mu L of the standard working solution with the gradient concentration prepared in the step (1), and uniformly mixing the standard working solution with the substrate of saxagliptin with the series of concentrations in a vortex manner;
(6) sample introduction detection: and (3) injecting the substrate standard working solution of the saxagliptin with the series of concentrations prepared in the step (4) and the sample injection product of the saxagliptin to be detected prepared in the step (3) into a liquid chromatograph, and detecting by a tandem mass spectrometer to obtain the content of the saxagliptin in the plasma.
The concentration gradient of the standard working solution in the step (1) is 0.1ng/mL, 1.5ng/mL, 10ng/mL, 20ng/mL, 40ng/mL, 50ng/mL, 80ng/mL and 100 ng/mL.
In the step (2) and the step (3), the vortex time is 2min, the vortex rotation speed at room temperature is 4500rpm, the centrifugation time is 10min, and the centrifugation speed is 13500 r/min.
The conditions of the liquid chromatogram determination in the step (5) are as follows: a chromatographic column: the chromatographic column is Waters BEH Shield RP18(ii) a Mobile phase: 10mmol/L ammonium acetate-acetonitrile (70: 30, V/V); flow rate: 0.3 mL/min; column temperature: 30 ℃; sample introduction amount: 10.0. mu.L.
The mass spectrum determination conditions of the step (5) are as follows: an ion source: ESI, positive ion mode; capillary voltage: 4.0 kv; ion source temperature: 110 ℃; the temperature of desolventizing gas is 350 ℃; desolventizing agent gas flow: 800L/hr; the cone hole blowback air flow is 50L/hr; taper hole voltage: 30 v; the scanning mode is as follows: positive ion Multiple Reaction Monitoring (MRM); ion pairing: 316.2/180.2.
And performing linear regression by taking the mass concentration (ng/mL) of the substance to be detected as an abscissa (X) and taking the peak area ratio of the substance to be detected to the internal standard as an ordinate (Y). As a result, the regression equation for saxagliptin was 4 × 10-3x-5.63 × 10-5(r ═ 0.9972), the linear range was 0.1 to 100ng/mL, and the lower limit of the quantification was 0.1ng/mL, respectively.
The foregoing is merely exemplary and illustrative of the present inventive concept and various modifications, additions and substitutions of similar embodiments may be made to the specific embodiments described by those skilled in the art without departing from the inventive concept or exceeding the scope of the claims as defined in the accompanying claims.
Claims (5)
1. A method for quantitative detection and analysis of saxagliptin is characterized by comprising the following steps: the method comprises the following steps:
(1) preparation of standard working solutions: precisely weighing a saxagliptin reference substance, dissolving and diluting the reference substance with 50% acetonitrile, and then diluting the reference substance with 10% methanol to obtain standard working solutions with 9 concentration gradients;
(2) preparation of internal standard solution: precisely weighing a saxagliptin reference substance, dissolving and diluting the reference substance with 50% acetonitrile to prepare an internal standard stock solution with the mass concentration of 1mg/mL, and then diluting the internal standard stock solution with 10% methanol to prepare an internal standard solution with the mass concentration of 50 ng/mL;
(3) plasma sample treatment: taking 100 mu L of plasma sample, putting the plasma sample into a 1.5mL centrifuge tube, respectively adding 50 mu L of 50ng/mL internal standard solution and 500 mu L of acetonitrile, and taking supernate after vortex and centrifugation;
(4) sample purification: transferring the supernatant obtained in the step (3) into a 1.5mL centrifuge tube, drying the centrifuge tube with nitrogen at room temperature, re-dissolving the residue with 200 mu L10% methanol, performing vortex and centrifugation, and then taking the supernatant to obtain a sample of saxagliptin to be detected for ultra performance liquid chromatography tandem mass spectrometry;
(5) matrix standard working solution: treating and purifying the blank plasma sample according to the steps (2) and (3), drying the blank plasma sample by blowing nitrogen, adding 10 mu L of the standard working solution with the gradient concentration prepared in the step (1), and uniformly mixing the standard working solution with the substrate of saxagliptin with the series of concentrations in a vortex manner;
(6) sample introduction detection: and (3) injecting the substrate standard working solution of the saxagliptin with the series of concentrations prepared in the step (4) and the sample injection product of the saxagliptin to be detected prepared in the step (3) into a liquid chromatograph, and detecting by a tandem mass spectrometer to obtain the content of the saxagliptin in the plasma.
2. The method for quantitative detection and analysis of saxagliptin according to claim 1, characterized in that: the concentration gradient of the standard working solution in the step (1) is 0.1ng/mL, 1.5ng/mL, 10ng/mL, 20ng/mL, 40ng/mL, 50ng/mL, 80ng/mL and 100 ng/mL.
3. The method for quantitative detection and analysis of saxagliptin according to claim 1, characterized in that: in the step (2) and the step (3), the vortex time is 2min, the vortex rotation speed at room temperature is 4500rpm, the centrifugation time is 10min, and the centrifugation speed is 13500 r/min.
4. The method for quantitative detection and analysis of saxagliptin according to claim 1, characterized in that: the conditions for measuring the liquid chromatogram in the step (5) are as follows: a chromatographic column: the chromatographic column is Waters BEH Shield RP18(ii) a Mobile phase: 10mmol/L ammonium acetate-acetonitrile (70: 30, V/V); flow rate: 0.3 mL/min; column temperature: 30 ℃; sample introduction amount: 10.0. mu.L.
5. The method for quantitative detection and analysis of saxagliptin according to claim 1, characterized in that: the mass spectrum measuring conditions in the step (5) are as follows: an ion source: ESI, positive ion mode; capillary voltage: 4.0 kv; ion source temperature: 110 ℃; the temperature of desolventizing gas is 350 ℃; desolventizing agent gas flow: 800L/hr; the cone hole blowback air flow is 50L/hr; taper hole voltage: 30 v; the scanning mode is as follows: positive ion Multiple Reaction Monitoring (MRM); ion pairing: 316.2/180.2.
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| CN111189949A (en) * | 2019-12-13 | 2020-05-22 | 大连市检验检测认证技术服务中心 | Method for simultaneously detecting linagliptin and saxagliptin in health food |
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- 2020-11-27 CN CN202011356263.8A patent/CN112326842A/en active Pending
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| US20160084848A1 (en) * | 2013-06-19 | 2016-03-24 | Weixun Wang | Assay for determining endogenous levels of analyte in vivo |
| CN106389453A (en) * | 2015-05-25 | 2017-02-15 | 蔡世珍 | Flavone glycoside composition |
| CN107045031A (en) * | 2017-04-26 | 2017-08-15 | 苏州海科医药技术有限公司 | The LC MS/MS high-flux detection methods of BMS-477118 and 5 hydroxyl BMS-477118s in human plasma |
| CN111189949A (en) * | 2019-12-13 | 2020-05-22 | 大连市检验检测认证技术服务中心 | Method for simultaneously detecting linagliptin and saxagliptin in health food |
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Application publication date: 20210205 |