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Method for detecting residual organic solvents in medicines by high performance liquid chromatography

A high-performance liquid chromatography, residual organic solvent technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of difficult detection and poor operability, and achieve the effects of accurate and reliable results and high detection sensitivity

Inactive Publication Date: 2014-07-16
CHENGDU CHEMPARTNER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The technical problem to be solved by the present invention is to overcome the residual N,N-dimethylformamide (DMF), N-N-dimethylacetamide (DMAC) and N-methylpyrrolidone (NMP) in the water-soluble drugs in the prior art The defects of difficult detection and poor operability provide a method for detecting residual organic solvents in drugs by high performance liquid chromatography (HPLC), which can accurately detect residual N,N- in water-soluble drugs Dimethylformamide (DMF), N-N-dimethylacetamide (DMAC) and N-methylpyrrolidone (NMP), convenient and fast, high sensitivity, can detect low concentration samples, and high accuracy

Method used

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  • Method for detecting residual organic solvents in medicines by high performance liquid chromatography
  • Method for detecting residual organic solvents in medicines by high performance liquid chromatography
  • Method for detecting residual organic solvents in medicines by high performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] 1. Preparation of mixed solvent standard solution and sample to be tested (such as fospropofol sodium drug sample) solution

[0057] 1. Preparation of mixed solvent standard solution (0.088mg / mL DMF, 0.109mg / mL DMAC and 0.053mg / mL NMP):

[0058] Weigh 88mg of DMF, 109mg of DMAC and 53mg of NMP into a 10mL volumetric flask containing 3mL of mobile phase A, dissolve with mobile phase A, dilute to the mark and mix well. Then precisely pipette 1.0mL of this solution into a 100mL volumetric flask, dilute to the mark with mobile phase A, shake well and prepare for sample injection, marked as STD#1 control solution;

[0059] Wherein, described mobile phase A is the NaH of 0.01mol / L 2 PO 4 buffer, the NaH 2 PO 4 The pH of the buffer was 6.0.

[0060] In order to check whether the preparation of standard 1 (STD#1) and its detection are reliable, STD#2 control solution was prepared in the same way.

[0061] 2. Preparation of the sample solution to be tested (fospropofol sod...

Embodiment 2

[0113] Chromatographic column: octane bonded silica gel column.

[0114] Mobile phase: mobile phase A: ammonium acetate, the pH of ammonium acetate is 5.8; mobile phase B: acetonitrile;

[0115] Flow rate: 0.5mL / min;

[0116] Column temperature: 30°C;

[0117] Detection wavelength: 230nm;

[0118] Injection volume: 5μL;

[0119] All the other operating steps and conditions are the same as in Example 1.

[0120] Through the above experimental steps, the contents of DMF, DMAC and NMP in the sample can be measured, and the detection results are accurate and reliable.

Embodiment 3

[0122] Chromatographic column: phenyl chromatographic column.

[0123] Mobile phase: mobile phase A: 0.01mol / L NaH 2 PO 4 Buffer (adjust pH to 10 with 0.1mol / L NaOH); mobile phase B: acetonitrile;

[0124] The mobile phase gradient conditions are as follows:

[0125] time min

NaH 2 PO 4 Buffer % (A%)

Acetonitrile% (B%)

0.0

90

10

5.0

90

10

10

10

90

20

10

90

20.0

stop

[0126] Flow rate: 1.5mL / min;

[0127] Column temperature: 20°C;

[0128] Detection wavelength: 240nm;

[0129] Injection volume: 5μL;

[0130] All the other operating steps and conditions are the same as in Example 1.

[0131] Through the above experimental steps, the contents of DMF, DMAC and NMP in the sample can be measured, and the detection results are accurate and reliable.

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Abstract

The invention discloses a method for detecting residual organic solvents in medicines by high performance liquid chromatography (HPLC). The method comprises a step of performing HPLC detection on a to-be detected sample subjected to pretreatment. Gradient elution is employed during detection, the mobile phase A is a buffer salt with a cut-off wavelength of 210 nm or less, and the mobile phase B is acetonitrile. Gradient elution is performed, specifically elution is performed for 5 min under the condition that the volume ratio of the mobile phase A to the mobile phase B is (90:10)-(98:2); then elution is performed under the condition that the volume ratio of the mobile phase A to the mobile phase B is (20:80)-(10:90), or linear elution is performed until the volume ratio of the mobile phase A to the mobile phase B is (20:80)-(10:90); and elution is finished until impurities are removed. The organic solvents are N,N-dimethylformamide, N,N-dimethylacetamide and N-methylpyrrolidinone. The method is capable of precisely detecting the above organic solvents, is convenient and rapid and high in sensitivity, and is capable of detecting low-concentration samples with high accuracy.

Description

technical field [0001] The invention relates to a method for detecting residual organic solvents in medicines by high performance liquid chromatography. Background technique [0002] N, N-dimethylformamide (N, N-dimethyl formamide, DMF) is a colorless organic solvent with a high boiling point, and its boiling point is 153°C. N,N-Dimethylformamide (DMF) is miscible with water, ethanol, ether, aldehydes, ketones, esters, halogenated hydrocarbons and aromatic hydrocarbons. Its structural formula is: [0003] [0004] Its molecular formula is: C 3 h 7 NO, molecular weight: 73.10 [0005] N,N-Dimethylacetamide (N,N-Dimethylacetamide, DMAC) is a colorless and transparent organic solvent with a boiling point of 166°C. It can be freely mixed with organic solvents such as water, alcohol, ether, ester, benzene, chloroform and aromatic compounds. Its structural formula is: [0006] [0007] Its molecular formula is: C 4 h 9 NO, molecular weight: 87.12 [0008] N-Methyl-...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 陈礼莉胡崇林李雯蒲友明
Owner CHENGDU CHEMPARTNER
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