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Method for determining residual solvent in phthalide compound

A technology for residual solvents and compounds, which is applied in the field of pharmaceutical analysis, can solve the problems of inability to detect n-heptane, etc., and achieve the effects of improving sample recovery, high sensitivity, and high accuracy

Active Publication Date: 2019-10-11
弘和制药有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

WS1-(X-124)-2005Z uses n-heptane as an internal standard, and cannot detect residual n-heptane in raw materials or intermediates

Method used

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  • Method for determining residual solvent in phthalide compound
  • Method for determining residual solvent in phthalide compound
  • Method for determining residual solvent in phthalide compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Chromatographic column: Agilent DB-624, 30m×0.530mm, 3μm.

[0063] FID detector temperature: 250°C, headspace inlet temperature: 220°C, N 2 Gas flow rate: 3.0ml / min, split ratio - 5:1, solvent: N-methylpyrrolidone.

[0064] Heating program: start at 40°C and hold for 5 minutes; heat up to 150°C at 8°C / min and hold for 2 minutes; then heat up to 220°C at 50°C / min.

[0065] Headspace temperature: 80°C, equilibration time: 30min, solvent: N-methylpyrrolidone, concentration of the test product: 0.1g / mL.

[0066] Preparation of 100% reference substance solution: Take an appropriate amount of residual solvent reference substance, and use N-methylpyrrolidone to prepare methanol, acetonitrile, dichloromethane, ethyl acetate, tetrahydrofuran and n-heptane 0.3mg / ml, 0.041mg / ml, The mixed solution of 0.06mg / ml, 0.5mg / ml, 0.072mg / ml and 0.5mg / ml, accurately measure 5.0ml into a 20ml headspace bottle, seal it, and it is 100% reference substance solution. The measured gas chromato...

Embodiment 2

[0074] Chromatographic column: Agilent DB-624, 30m×0.530mm, 3μm.

[0075] FID detector temperature: 250°C, headspace inlet temperature: 220°C, N 2 Gas flow rate: 3.0ml / min, split ratio - 5:1, solvent: N-methylpyrrolidone.

[0076] Heating program: start at 40°C and hold for 5 minutes; heat up to 150°C at 8°C / min and hold for 2 minutes; then heat up to 220°C at 50°C / min and hold for 3 minutes. Headspace temperature: 80°C, equilibration time: 30min, solvent: N-methylpyrrolidone, concentration of the test product: 0.1g / mL.

[0077] Preparation of 100% reference substance solution: Take an appropriate amount of residual solvent reference substance, and use N-methylpyrrolidone to prepare methanol, acetonitrile, dichloromethane, ethyl acetate, tetrahydrofuran and n-heptane 0.3mg / ml, 0.041mg / ml, The mixed solution of 0.06mg / ml, 0.5mg / ml, 0.072mg / ml and 0.5mg / ml, accurately measure 5.0ml into a 20ml headspace bottle, seal it and ultrasonicate at 40kHz for 5 minutes, it is a 100% ref...

Embodiment 3

[0115] The chromatographic conditions are as follows:

[0116] Chromatographic column: Agilent DB-624, 30m×0.530mm, 3μm.

[0117] FID detector temperature: 250°C, headspace inlet temperature: 220°C, N 2 Gas flow rate: 3.0ml / min, split ratio - 5:1, solvent: N-methylpyrrolidone.

[0118] Heating program: start at 40°C and hold for 5 minutes; heat up to 150°C at 8°C / min and hold for 2 minutes; then heat up to 220°C at 50°C / min and hold for 3 minutes. Headspace temperature: 80°C, equilibration time: 30min, solvent: N-methylpyrrolidone, concentration of the test product: 0.1g / mL. The test product was sealed after the headspace bottle was displaced, and ultrasonicated at 40kHz for 5 minutes.

[0119] Reference substance configuration: N-methylpyrrolidone was used to prepare methanol, acetonitrile, dichloromethane, ethyl acetate, tetrahydrofuran and n-heptane 0.3mg / ml, 0.041mg / ml, 0.06mg / ml, 0.5mg / ml, 0.072mg / ml, 0.5mg / ml mixed solution, accurately measure 5.0ml into a 20ml heads...

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Abstract

A gas chromatographic method for determining a residual solvent in a phthalide compound takes cyanopropyl phenyl-dimethyl polysilicone as a stationary liquid capillary chromatographic column, hydrogenas a flame ionization detector and nitrogen as a carrier gas and calculates content of the residual solvent in peak area according to an external standard process. The method can determine normal heptane and other residual solvents in the phthalide compound and has the advantages of high sensitivity, strong specificity and high accuracy.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a gas chromatography method for determining residual solvents in phthalide compounds. Background technique [0002] Phthalide is also known as o-hydroxymethylbenzoic acid lactone. Existing studies have shown that many phthalide compounds have pharmacological activity and can be applied to the prevention or treatment of cardiovascular and cerebrovascular diseases. Butylphthalide is the third new chemical entity drug independently researched and developed in my country. The medicinal salt of 2-(α-hydroxypentyl)benzoic acid has entered the clinical development stage. It has been reported in the literature that 3-butenylphthalide has the ability to inhibit thrombosis. Alkanes synthesis activity, in addition, 3-(3'-hydroxy)-butylphthalide, 3-hydroxy-3-butylphthalide (also known as 3-n-butyl-3-hydroxy-1(3H)-isobenzo Furanones) are butylphthalide compounds with pharmacological activity. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/68G01N30/86G01N30/04G01N30/06G01N30/60
CPCG01N30/02G01N30/68G01N30/8634G01N30/04G01N30/06G01N30/60G01N2030/047
Inventor 孙明君李钦刘严王芷陈文斯胡金
Owner 弘和制药有限公司
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