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Method for screening acid drugs in liquid medicines by coupling solid phase extraction-liquid chromatography

A liquid drug and liquid chromatography technology, applied in the field of drug analysis, can solve problems such as poor resolution of target products, late peaking time, and long test time.

Active Publication Date: 2017-10-27
河北八和科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is suitable for the separation of several non-steroidal anti-inflammatory drugs in water, but not suitable for emulsion samples. The existing problems are that the resolution of some target products is not good, the peak shape of some target products is not good, and the overall The peak time is later, requiring a longer test time

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  • Method for screening acid drugs in liquid medicines by coupling solid phase extraction-liquid chromatography
  • Method for screening acid drugs in liquid medicines by coupling solid phase extraction-liquid chromatography
  • Method for screening acid drugs in liquid medicines by coupling solid phase extraction-liquid chromatography

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Embodiment 1

[0022] A method for screening acidic drugs in liquid drugs by solid-phase extraction-liquid chromatography, comprising the following steps:

[0023] Preparation of standard samples, preparing single and mixed standards of meloxicam, ketoprofen, indomethacin, diclofenac, and gemfibrozil; through full-band scanning of diode array detectors, to determine the detection of each substance Wavelength; Determination of standard curve.

[0024] For the pretreatment of the test sample, add anhydrous calcium chloride and acetonitrile / phosphoric acid solution to the emulsion sample for separation; take 5ml emulsion sample, add 0.5g of anhydrous calcium chloride, and add a volume ratio of 50:1 acetonitrile / phosphoric acid The amount of phosphoric acid solution was 5ml for extraction, and the supernatant was obtained by centrifugation.

[0025] Self-made solid phase extraction column,

[0026] Take 0.5g of 50-150μm neutral alumina, add 1.0g of 150-250μm Flory diatomaceous earth, add 15ml ...

Embodiment 2

[0034] The difference from Example 1 is that 5ml of the emulsion sample is taken, 1.5g of anhydrous calcium chloride is added, and 10ml of acetonitrile / phosphoric acid solution with a volume ratio of 150:1 is added for extraction, and the supernatant is obtained by centrifugation. The mobile phase B is acetonitrile: 5% tetramethylammonium hydroxide: water (600:10:1000), and the flow rate of the mobile phase is 2ml / min.

Embodiment 3

[0036] The difference with Example 1 is that, the difference with Example 1 is that the 5ml emulsion sample is taken, the amount of calcium chloride anhydrous is added 1.0g, and the volume ratio of adding is 100:1 acetonitrile / phosphoric acid solution amount is 7.5ml was extracted and centrifuged to obtain the supernatant. The mobile phase B is acetonitrile: 5% tetramethylammonium hydroxide: water (500:10:1000), and the mobile phase flow rate is 1.5ml / min.

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Abstract

The invention discloses a method for screening acid drugs in liquid medicines by coupling solid phase extraction-liquid chromatography. The method comprises the following steps: preparing a standard sample, and preparing the single and mixed standard sample of meloxicam, ketoprofen, indomethacin, diclofenac and gemfibrozil; preprocessing a test sample, adding anhydrous calcium chloride and acetonitrile / phosphoric acid solution into the sample for extraction, and carrying out separation to obtain supernate; carrying out solid phase extraction column purification, processing the supernate by the solid phase extraction column of aluminium oxide and kieselguhr mixed filler to obtain the test sample; carrying out efficient liquid phase chromatography detection, and detecting the single and mixed standard sample and a test sample. The method is suitable for emulsion samples, various ingredients are simultaneously detected, and the method has the advantages of high degree of separation, high appearance time and high recovery rate.

Description

technical field [0001] The invention relates to the field of drug analysis, in particular to a method for screening acidic drugs in liquid drugs by combining solid phase extraction and liquid chromatography. Background technique [0002] Solid Liquid Extraction (Solid Liquid Extraction, SLE) is a physical extraction process including liquid phase and solid phase. During the extraction process, when the sample passes through the solid phase column, the analyte is adsorbed on the surface of the solid packing, and other sample components are analyzed through the column. The substance can be eluted with an appropriate solvent, so as to achieve the purpose of separation and purification. Solid-phase extraction is a pre-sample processing technology. It has two functions in sample processing: one is purification and the other is enrichment. These two functions can exist at the same time. Since it was developed in the 1970s, it has been widely used in laboratories. Solid-phase ext...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06
CPCG01N30/06G01N2030/062
Inventor 巩克民孟丽季宏建
Owner 河北八和科技发展有限公司
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