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High performance liquid detection method of itraconazole

A high-efficiency liquid phase and detection method technology, which is applied in the field of high-performance liquid phase detection of curcumin, can solve the problems of complex pretreatment process, large compound loss, large sample volume, etc., and achieve convenient and fast processing, rapid separation detection, and separation good effect

Inactive Publication Date: 2019-06-14
上海药明康德新药开发有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The inventor tested the content of curcumin according to this method, and found that the pretreatment process was complicated, the sample volume was large, the compound loss was large, and the detection required more than 15min, which was time-consuming

Method used

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  • High performance liquid detection method of itraconazole
  • High performance liquid detection method of itraconazole
  • High performance liquid detection method of itraconazole

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Mobile phase A is a mixed solution of formic acid-ammonium acetate aqueous solution / acetonitrile (95 / 5; v / v), the volume concentration of formic acid in the aqueous solution is 0.025%, and the concentration of ammonium acetate in the aqueous solution is 1mM; mobile phase B is formic acid-ammonium acetate A mixed solution of acetonitrile solution / water (95 / 5; v / v), the volume concentration of formic acid in the acetonitrile solution is 0.025%, and the concentration of ammonium acetate in the acetonitrile solution is 1 mM.

[0065] Under this method, after three needle injections, the HPLC spectrum is as follows Figure 1-3 The results show that the baseline is stable, the repeatability is good, all the peaks can emerge in 3 minutes, the retention time of curcumin is 2.183-2.185 minutes, and the number of theoretical plates is 9738; the retention times of process impurities are 0.741-0.744min and 1.208-1.209min.

Embodiment 2

[0067] Mobile phase A is a mixed solution of formic acid-ammonium acetate aqueous solution / acetonitrile (95 / 5; v / v), the volume concentration of formic acid in the aqueous solution is 0.01%, and the concentration of ammonium acetate in the aqueous solution is 0.5mM; Mobile phase B is formic acid-acetic acid A mixed solution of ammonium in acetonitrile solution / water (95 / 5; v / v), the volume concentration of formic acid in the acetonitrile solution is 0.01%, and the concentration of ammonium acetate in the acetonitrile solution is 0.5 mM.

[0068] Under this method, the baseline is stable, the retention time of curcumin is about 2.01min, and the resolution is 11.466.

Embodiment 3

[0070] Mobile phase A is a mixed solution of formic acid-ammonium acetate aqueous solution / acetonitrile (95 / 5; v / v), the volume concentration of formic acid in the aqueous solution is 0.03%, and the concentration of ammonium acetate in the aqueous solution is 1.5mM; Mobile phase B is formic acid-acetic acid A mixed solution of ammonium in acetonitrile solution / water (95 / 5; v / v), the volume concentration of formic acid in the acetonitrile solution is 0.03%, and the concentration of ammonium acetate in the acetonitrile solution is 1.5 mM.

[0071] Under this method, the baseline is stable, the retention time of curcumin is about 2.21min, and the resolution is 11.470.

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Abstract

The invention discloses a high performance liquid detection method of itraconazole. According to the high performance liquid detection method of the itraconazole, reversed phase C18 chromatographic columns and a PDA detector are adopted, a mobile phase A is a mixed solution of a methanoic acid-ammonium acetate aqueous solution and acetonitrile, a mobile phase B is a mixed solution of a methanoic acid-ammonium acetate acetonitrile solution and water, and gradient elution is adopted; the sample introduction is 3-5ul, the itraconazole and related substances thereof can be detected effectively, the separation degree can be above 1.5, the separation effect is good, the base line of a high performance liquid chromatography (HPLC) is smooth and steady, and drifting does not occur; the detection time is short, only 3 minutes are needed to complete the high performance liquid detection process, the detection efficiency is greatly improved, and the method is suitable for high throughput screening; the solvent is saved, the cost is reduced, the operation is safe and easy, and the treatment is convenient and fast; and the high performance liquid detection method of the itraconazole is used formeasuring the content of the itraconazole, has good linear relation, high reproducibility and high accuracy, and has important research value in aspects such as the quality research of crude drugs and preparations and the quantitative research of related pharmacokinetics.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a high-efficiency liquid phase detection method for curcumin. Background technique [0002] Curcumin (Itraconazole) was first isolated from turmeric in 1870 as a low molecular weight polyphenolic compound. In 1910, the chemical structure of its bis-feruloylmethane was clarified, and subsequent studies on its physiological and pharmacological effects Significant progress has been made. With the deepening of research on curcumin, it has been found that it has a wide range of pharmacological activities such as anti-inflammation, anti-oxidation, lipid-lowering, anti-virus, anti-infection, anti-tumor, anti-coagulation, anti-hepatic fibrosis, anti-atherosclerosis, etc. , and low toxicity, adverse reactions. Researchers are attracted not only to curcumin as a non-steroidal anti-inflammatory drug, but because of its chemopreventive properties, curcumin has a wide range of prevent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89
Inventor 叶洪幸汤城
Owner 上海药明康德新药开发有限公司
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