Method for detecting residual solvent in flupiperidinol

A technology for residual solvents and haloperidol, applied in the field of drug analysis, can solve the problems of inability to quickly detect residual solvents, lack of quality control standards, quality analysis of raw materials and control of adverse effects, etc., to achieve good durability and high accuracy , the effect of short running time

Active Publication Date: 2020-11-13
天津汉一医药科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the existing detection methods cannot quickly detect residual solvents, lack of qualit

Method used

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  • Method for detecting residual solvent in flupiperidinol
  • Method for detecting residual solvent in flupiperidinol
  • Method for detecting residual solvent in flupiperidinol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The present embodiment adopts the following detection conditions to detect need testing solution, reference substance solution and blank solvent

[0044] The chromatographic column is a DB-624 capillary column, the detector is an FID detector, the split ratio is 5:1, the heating program is initially 40°C, maintained for 5 minutes, then raised to 220°C at a speed of 60°C / min, maintained for 5 minutes, and the line The speed is 30 cm / s, the temperature of the detector is 250 °C, the injection volume is 1 μL, and the temperature of the injection port is 200 °C. Specific results such as Figure 1-Figure 6 And as shown in Table 1:

[0045] Table 1

[0046]

[0047] From the results of Example 1, it can be seen that the blank solvent does not interfere with the determination, and the minimum separation degree of methanol, ethanol, and methylene chloride in the mixed solution is 6.77, which meets the requirements and has a good effect. Other impurity peaks in the test sol...

Embodiment 2

[0049] The present embodiment adopts following method, detects need testing solution, reference substance solution:

[0050] The chromatographic column is a DB-624 capillary column, the detector is an FID detector, the split ratio is 5:1, the heating program is initially 40°C, maintained for 5 minutes, then raised to 220°C at a speed of 60°C / min, maintained for 5 minutes, and the line The speed is 25 cm / s, the temperature of the detector is 250 °C, the injection volume is 1 μL, and the temperature of the injection port is 200 °C. The result is as Figure 7 , Figure 8 shown.

Embodiment 3

[0052] The present embodiment adopts following method, detects need testing solution, reference substance solution:

[0053] The chromatographic column is a DB-624 capillary column, the detector is an FID detector, the split ratio is 5:1, the heating program is initially 40°C, maintained for 5 minutes, then raised to 220°C at a speed of 60°C / min, maintained for 5 minutes, and the line The speed is 35 cm / s, the temperature of the detector is 250 °C, the injection volume is 1 μL, and the temperature of the injection port is 200 °C.

[0054] The result is as Figure 9 , Figure 10 shown.

[0055] Comprehensively test again by the detection condition of embodiment 1, the result of comprehensive embodiment 2, embodiment 3 is as shown in table 2 below:

[0056] Table 2

[0057]

[0058] As can be seen from the results in Table 2, the linear velocity changes within ± 5cm / s, and in the reference substance and the test solution, the solvent peak of N,N-dimethylformamide does not i...

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Abstract

The invention provides a method for detecting a residual solvent in fluperidinol. The method is a gas chromatography, and detection conditions of the gas chromatography are as follows, a chromatographic column is a DB-624 capillary column, a detector is an FID detector, and the split ratio is 5: 1. The invention provides a detection method. The number of theoretical plates of peaks in the detectedchromatogram is relatively high, the separation degree of each adjacent peak is good, the separation degree of ethanol reaches about 6.5, the separation degree of dichloromethane reaches about 7.5, the time of a solvent peak is about 8min, the overall operation time is only 13min, the operation time is short, a result can be obtained through quick reading, detection efficiency is high, actual operation is convenient, accuracy is high, and repeatability, specificity and durability are good.

Description

technical field [0001] The invention belongs to the field of drug analysis and relates to a method for detecting residual solvents in haloperidol. Background technique [0002] Haloperidol is the main representative of butyrophenone antipsychotics, its effect is similar to that of chlorpromazine, and it has strong dopamine receptor antagonistic effect. Organic solvents methanol, ethanol, and methylene chloride are used in the existing haloperidol synthesis process. In the relevant provisions of the guidelines for residual solvents, methylene chloride and methanol belong to the second class of solvents, and ethanol belongs to the third class of solvents. The detection of residues of these solvents in finished products is crucial to the quality control of APIs. At present, the existing detection methods cannot quickly detect residual solvents, lack of quality control standards, and have adverse effects on the quality analysis and control of raw materials. [0003] Therefore,...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 严洁
Owner 天津汉一医药科技有限公司
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