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A kind of assay method of everolimus intermediate

A determination method and everolimus technology, which is applied in the field of substance content determination, can solve problems such as undocumented intermediate content determination methods, and achieve the effects of stable and reliable results, good repeatability and durability, and simple operation.

Active Publication Date: 2020-03-31
SHANDONG NEWTIME PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although patents WO2012103959A1 and CN101175760A describe the analysis methods of everolimus and rapamycin-related derivatives, they do not describe the content determination method of the intermediate, and the determination of the content of the intermediate is based on the quality of the intermediate product. The control process and even the quality control process of everolimus play a very important role, so it is necessary to establish a stable and effective assay method for the quality control of this intermediate

Method used

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  • A kind of assay method of everolimus intermediate
  • A kind of assay method of everolimus intermediate
  • A kind of assay method of everolimus intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Instruments and conditions: Agilent 1260 liquid chromatography system, DAD detector, chromatographic column: Agilent, SB-C18 applicable; 4.6×250mm, 5μm, detection wavelength 277nm, column temperature 60°C, flow rate 1.0mL / min, mobile phase: volume The ratio of 0.02mol / L ammonium dihydrogen phosphate solution to methanol is 8:92.

[0033] Experimental procedure: dissolve the everolimus intermediate with acetonitrile and quantitatively dilute it to make a solution containing 0.5 mg of the everolimus intermediate per 1 mL, as the test solution, accurately measure 10 μL of the test solution and inject it into the liquid phase Chromatograph, carry out high-performance liquid chromatography analysis according to the above conditions, record the chromatogram, the results are shown in the attached figure 1 .

[0034] attached figure 1 It shows that under the chromatographic conditions, the everolimus intermediate peak and the impurity peak can be completely separated, and the...

Embodiment 2

[0036] Instruments and conditions: Agilent 1260 liquid chromatography system, DAD detector, chromatographic column: Agilent, SB-C18 applicable; 4.6×250mm, 5μm, detection wavelength 277nm, column temperature 60°C, flow rate 0.7mL / min, mobile phase: volume The ratio of 0.01mol / L ammonium dihydrogen phosphate solution to methanol is 5:95.

[0037] Experimental procedure: dissolve the everolimus intermediate with methanol and quantitatively dilute it to make a solution containing 0.5 mg of the everolimus intermediate per 1 mL, as the test solution, accurately measure 10 μL of the test solution and inject it into the liquid phase Chromatograph, carry out high-performance liquid chromatography analysis according to the above conditions, record the chromatogram, the results are shown in the attached figure 2 .

[0038] attached figure 2 It shows that under the chromatographic conditions, the everolimus intermediate peak and the impurity peak can be completely separated, and the r...

Embodiment 3

[0040] Instruments and conditions: Agilent 1260 liquid chromatography system, DAD detector, chromatographic column: Agilent, SB-C18 applicable; 4.6×250mm, 5μm, detection wavelength 277nm, column temperature 60°C, flow rate 1.2mL / min, mobile phase: volume The ratio of 0.04mol / L ammonium dihydrogen phosphate solution to methanol is 15:85.

[0041] Experimental procedure: dissolve the everolimus intermediate with acetonitrile and quantitatively dilute it to make a solution containing 0.5 mg of the everolimus intermediate per 1 mL, as the test solution, accurately measure 10 μL of the test solution and inject it into the liquid phase Chromatograph, carry out high-performance liquid chromatography analysis according to the above conditions, record the chromatogram, the results are shown in the attached image 3 .

[0042] attached image 3 It shows that under the chromatographic conditions, the everolimus intermediate peak and the impurity peak can be completely separated, and th...

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Abstract

The invention relates to an everolimus-intermediate content determination method. The method is used for quality control of an everolimus intermediate, octadecylsilane chemically bonded silica serves as a chromatographic column (C18, 4.6*250 mm, 5 microns) of filler, a buffer salt solution and methyl alcohol serve as a moving phase, the detection wave length ranges from 272 nm to 282 nm, the column temperature ranges from 55 DEG C to 65 DEG C, and content determination is carried out with the high-performance liquid chromatography method. By means of the content determination method, the everolimus intermediate can be effectively separated from impurities of the everolimus intermediate, and the method has the advantages of being high in sensitivity and separation degree, easy to operate, good in repeatability and durability and stable and reliable in result.

Description

technical field [0001] The invention relates to a method for determining the content of a substance, in particular to a method for determining the content of an everolimus intermediate. Background technique [0002] Everolimus (everolimus) is a new generation of macrolide rapamycin derivative drugs. The drug was developed by Novartis Corp. and first launched in Germany in 2004. It is mainly used for 1) advanced renal cancer that is ineffective for other drugs; 2) it can supplement the immunosuppression of calcineurin inhibitor cyclosporine It is used to prevent the rejection of heart or kidney transplantation; 3) Drug-eluting stent drug is one of the most commonly used drugs for drug-eluting stents. [0003] (3S,6R,7E,9R,10R,12R,14S,15E,17E,19E,21S,23S,26R,27R,34aS)-9,10,12,13,14,21,22,23,24, 25,26,27,32,33,34,34a-Hexadecahydro-9-trimethylsilyloxy-27-hydroxy-3-[(1R)-2-[(1S,3R,4R)-4 -Hydroxy-3-methoxycyclohexyl]-1-methylethyl]-10,21-dimethoxy-6,8,12,14,20,26-hexamethyl-23,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 张贵民颜凯赵亮亮
Owner SHANDONG NEWTIME PHARMA