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Detection method of 1-[2-(2, 4-dimethylphenylthioalkyl)phenyl]piperazine or salt thereof

A technology of dimethylphenylsulfanyl and detection method, which is applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve the problems of difficult separation, difficult separation of isomers and vortioxetine, etc., and achieve separation Good quality, good for quality control, stable baseline

Active Publication Date: 2017-04-05
四川弘远药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to reports, there are nearly 20 impurities related to vortioxetine, some of which are very similar in structure and polarity to vortioxetine, and it is difficult to separate them in the actual detection process
How to separate each impurity from the main component and effectively solve the problem of difficult separation of isomers and vortioxetine has become an urgent problem to be solved

Method used

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  • Detection method of 1-[2-(2, 4-dimethylphenylthioalkyl)phenyl]piperazine or salt thereof
  • Detection method of 1-[2-(2, 4-dimethylphenylthioalkyl)phenyl]piperazine or salt thereof
  • Detection method of 1-[2-(2, 4-dimethylphenylthioalkyl)phenyl]piperazine or salt thereof

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Experimental program
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preparation example Construction

[0046] Solution preparation:

[0047] Impurity mixed control solution: Accurately weigh the appropriate amount of impurity E, I, K, and L reference substances, add methanol to dissolve and dilute to make a concentration of about 1mg·mL -1 The impurities mixed with the control solution.

[0048] The test solution: take a sample of vortioxetine hydrobromide, dissolve it in methanol and quantitatively dilute it to make a concentration of 10.0036mg·mL -1 The solution, as the stock solution of the test sample, was quantitatively diluted 10 times, as.

[0049] Mixed test solution: mix the above-mentioned impurity mixed control solution with vortioxetine hydrobromide test solution as the test solution for specificity investigation.

Embodiment 1

[0051] The chromatographic conditions used Waters Xselect HSS PFP column (150mm×4.6mm, 5μm), mobile phase A was methanol-0.02mol L -1 Ammonium acetate buffer solution (containing 0.5% triethylamine, adjusted to pH 4.0 with acetic acid) (20:80), mobile phase B is acetonitrile, gradient elution, as shown in the table below.

[0052]

[0053] The detection wavelength is 254nm, the column temperature is 35°C, the flow rate is 1.0mL·min-1, and the injection volume is 10-20μL.

[0054] Get the reference substance, the test solution and the mixed test solution to carry out liquid chromatography detection respectively, wherein the separation between vortioxetine and the adjacent impurity peaks and the rest of the impurities in the mixed test solution is good, and the test results are shown in figure 1 .

Embodiment 2

[0056]Chromatographic conditions: chromatographic column Agilent C185μm column (250mm×4.6mm, 5μm), the mobile phase is acetonitrile-0.07mo / L ammonium formate solution (88:12), the detection wavelength is 240nm; the column temperature is 30°C; the flow rate is 1mL min -1 ; The injection volume is 10-20 μl.

[0057] Get reference substance, need testing solution and mixed test solution to carry out liquid chromatography detection respectively, wherein test solution carries out liquid chromatography detection, and detection result sees figure 2 .

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Abstract

The invention provides a detection method of 1-[2-(2, 4-dimethylphenylthioalkyl)phenyl]piperazine or salt thereof. The method includes the steps of: taking a methanol solution containing 1-[2-(2, 4-dimethylphenylthioalkyl)phenyl]piperazine or salt thereof as a test solution, and performing detection according to high performance liquid chromatography conditions, which specifically includes: use of pentafluorophenyl as the filler; employment of a methanol-0.02mol.L<-1> ammonium acetate buffer solution as the mobile phase A, and taking of acetonitrile as the mobile phase B; and conducting gradient elution. The detection method has the advantages of good separation degree of active components and impurities, stable baseline, and good repeatability and stability of a sample and impurities, thus being more beneficial to quality control.

Description

technical field [0001] The invention relates to the field of drug detection, in particular to a detection method for 1-[2-(2,4-dimethylphenylsulfanyl)phenyl]piperazine or a salt thereof. Background technique [0002] 1-[2-(2,4-Dimethylphenylsulfanyl)phenyl]piperazine (vortioxetine) is jointly developed by Lundheck and Takeda Pharmaceutical Company, in which its hydrobromide (vortioxetine Tin hydrobromide) was approved by the U.S. Food and Drug Administration (FDA) on September 30, 2013 for the treatment of adult depression (MDD), mainly by increasing serotonin (5-serotonin) in the central nervous system (CNS). -HT) concentration exerts antidepressant effect. A number of clinical trials have shown that vortioxetine has good efficacy, safety and tolerability for the treatment of MDD. [0003] In drug research, not only the content control of active ingredients, but also the control of impurity content is becoming more and more strict. Impurity control is an important content...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/74G01N30/06
CPCG01N30/06G01N30/74
Inventor 柯潇林楠宋光华张伟孔祥瑞
Owner 四川弘远药业有限公司
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