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Detecting method for high performance liquid chromatography-tandem mass spectrometry of PDE5 type inhibitors in drugs, healthcare products and food

A high-performance liquid chromatography and tandem mass spectrometry technology is applied in the field of high-performance liquid chromatography-tandem mass spectrometry detection of PDE5 inhibitors, and can solve the problems of sildenafil, aminotadalafil, tadalafil, sulfur Substitute for idenafil, pseudo-vardenafil and other problems to achieve excellent qualitative ability and improve detection efficiency

Active Publication Date: 2012-07-04
广东省药品检验所
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The purpose of the invention is to overcome the existing liquid chromatography mass spectrometry technology to detect PDE in Chinese patent medicines. 5 Defects of type inhibitors, provide a kind of covering drug, health food and food in reddenafil, reddenafil, vardenafil, hydroxyhomosildenafil, sildenafil, homemoxicillin Eleven kinds of PDEs including Nafil, Aminotadalafil, Tadalafil, Thioedenafil, Pseudovardenafil and Namoxidenafil 5 Confirmation and Arbitration Method of Type Inhibitors by Liquid Chromatography-Tandem Mass Spectrometry (HPLC-MS / MS)

Method used

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  • Detecting method for high performance liquid chromatography-tandem mass spectrometry of PDE5 type inhibitors in drugs, healthcare products and food
  • Detecting method for high performance liquid chromatography-tandem mass spectrometry of PDE5 type inhibitors in drugs, healthcare products and food
  • Detecting method for high performance liquid chromatography-tandem mass spectrometry of PDE5 type inhibitors in drugs, healthcare products and food

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Experimental program
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Effect test

Embodiment 1

[0038] Embodiment 1: eleven kinds of PDE 5 HPLC-MS / MS detection method of type inhibitors

[0039] 1. Preparation of reference solution Aminotadalafil, pseudovardenafil, thioedenafil, and reddenafil reference substance about 10mg, put in a 50ml measuring bottle, dissolve with acetonitrile and dilute to the mark, shake well, and use 50% acetonitrile The solution is diluted to make a solution containing 5 μg per 1 ml, that is to say.

[0040] 2. Preparation of the test solution If the test product is a solid preparation, accurately weigh the dosage for one dose, grind it finely and transfer it to a 50ml measuring bottle, add about 40ml of acetonitrile, sonicate for 15 minutes, cool to room temperature, and dilute with acetonitrile to the mark, shake well, and filter; if the test product is a liquid preparation, accurately measure the dose for one time, put it in a 50ml measuring bottle, add about 40ml of acetonitrile, shake for 3 minutes, dilute with acetonitrile to the mark, ...

Embodiment 2

[0056] Embodiment 2, eleven kinds of PDE of the present invention method 5 Inhibitor Sensitivity and Sample Detection Results

[0057] In the present invention, the absolute mass of the components corresponding to three times the baseline noise is used as the detection limit, and the PDE 5 The detection limit of the type inhibitors was not more than 10ng. Reference PDE 5 The clinical effective dose of Nafil type inhibitor is 50~100mg, and Nafil is 5~20mg, adds the sample more than the effective dose, gets oral dose once and detects by the method for the embodiment of the present invention 1, through 100,000 times Injection after dilution can still be accurately and qualitatively detected. The sensitivity of the invention is sufficient to meet the needs of analysis.

[0058] Using the method of the present invention to detect and analyze 194 samples collected between 2006 and 2008, 132 samples were detected to be illegally added PDE 5 type inhibitor; added PDE 5 Type inhi...

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Abstract

The invention discloses a detecting method for high performance liquid chromatography-tandem mass spectrometry of PDE5 type inhibitors in drugs, healthcare products and food. Acetonitrile is used as extractant. 50 percent of acetonitrile is used as diluent. A formic acid-ammonium acetate solution-methanol-acetonitrile system is used as a flowing phase. With a flowing speed of 0.2-0.4 ml / min and a column temperature of 20-50 DEG C, liquid chromatographic column performs separation, then electrospray ionization (ESI) ion source is adopted for ionization, a positive ion mode is adopted for fully scanning a primary and a secondary mass spectrum, and whether the PDE5 type inhibitors is added in a sample can be qualitatively judged according to the secondary mass spectrum. The detecting method has simple sample pretreatment, high accuracy, good specificity, high detection flexibility and short analysis period, can accomplish qualitative analysis of 11 PDE5 type inhibitors through one experiment, is suitable for microscale analysis of the PDE5 type inhibitors and can be used as a verification and arbitration method for supervision inspection.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography-tandem mass spectrometry detection method, in particular to PDE in medicine, health food and food 5 A new technique for the detection of type inhibitors by high performance liquid chromatography-tandem mass spectrometry. Background technique [0002] Illegal addition of chemical ingredients in Chinese patent medicines for nourishing kidney and strengthening yang, health food and food is becoming more and more rampant, and there are more and more high-tech counterfeiting activities aimed at standards, which seriously threaten the health of the people. Such illegal activities are especially the illegal addition of PDE in Chinese patent medicines, health foods and foods with the effect of nourishing the kidney and strengthening yang. 5 Type inhibitor (phosphodiesterase type-5 inhibitor, phosphodiesterase type-5 inhibitor) is the most typical active. PDEs 5 PDE5 inhibitors are currently t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/28G01N30/72
Inventor 罗卓雅李延志李晨辉雷毅杨德忠
Owner 广东省药品检验所
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