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Method for separation and determination of raltitrexed and its enantiomers by high performance liquid chromatography

A technology of high performance liquid chromatography and enantiomers, which is applied in the field of pharmaceutical analysis to achieve good separation effect, accurate separation and quality control

Active Publication Date: 2019-11-01
NANJING CHIA TAI TIANQING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] There is no literature report on the separation and determination of raltitrexed and its enantiomers by high performance liquid chromatography

Method used

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  • Method for separation and determination of raltitrexed and its enantiomers by high performance liquid chromatography
  • Method for separation and determination of raltitrexed and its enantiomers by high performance liquid chromatography
  • Method for separation and determination of raltitrexed and its enantiomers by high performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1 specificity test

[0034] Instrument: Shimadzu LC-20AT high performance liquid chromatography

[0035] Detector: VWD

[0036] Workstation: Empower 3 software

[0037] Chromatographic column: Daicel CHIRALPAK AD-H (4.6mm×250mm, 5μm)

[0038] Detection wavelength: 226nm

[0039] Flow rate: 1.0ml / min

[0040] Column temperature: 35°C

[0041] Injection volume: 10μL

[0042] Mobile phase: n-hexane: 0.1% trifluoroacetic acid ethanol solution (55:45)

[0043] Blank: Methanol

[0044] Raltitrexed enantiomer reference substance stock solution: Take about 12.5 mg of raltitrexed enantiomer reference substance, accurately weighed, put in a 100ml measuring bottle, add about 50ml of methanol, and dissolve it by ultrasonic, Allow to cool to room temperature, dilute to volume with methanol, shake well, and obtain. (about 125μg / mL)

[0045] Raltitrexed enantiomer localization solution: Accurately measure 1.0 mL of raltitrexed enantiomer stock solution, put it in ...

Embodiment 2

[0049] Embodiment 2 durability test

[0050] On the basis of the detection chromatographic conditions in Example 1, the conditions such as the ratio of mobile phase, column temperature, flow rate, and wavelength were changed to investigate the durability of the enantiomer detection method.

[0051] Solution preparation and assay method are with reference to embodiment 3, and each chromatographic condition is shown in the table below:

[0052]

[0053] The results are shown in the table below:

[0054]

[0055] Conclusion: Under different chromatographic conditions, the peaks of raltitrexed and the enantiomers can be separated by baseline, and the resolution meets the requirements. The method has good durability.

Embodiment 3

[0056] Embodiment 3 detection limit test

[0057] Dilute the raltitrexed isomer localization solution with 0.1mol / L sodium hydroxide aqueous solution to prepare a series of low concentration solutions, and inject samples separately until S / N≥3, which is the detection limit. Results The detection limit of enantiomer was 5.87ng / mL.

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Abstract

The invention discloses a method for separation and determination of Raltitrexed and enantiomers of the Raltitrexed by high performance liquid chromatography. Tris(3,5-dimethylphenyl)-carbamate amylose is taken as a filler for a chiral chromatographic column, and a n-hexane-low alcohol solution is taken as a mobile phase, wherein the low alcohol solution contains trifluoroacetic acid with the concentration being 0.05-0.5%. The method is simple in operation and can rapidly and accurately separate and determine enantiomeric impurities in Raltitrexed bulk medicine and preparations of the Raltitrexed bulk medicine, thereby ensuring the quality controllability of the Raltitrexed.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for separating and measuring raltitrexed and its enantiomers through high-performance liquid chromatography. Background technique [0002] Raltitrexed was developed by the Cancer Research Unit at the Royal Marsden Hospital in the UK in collaboration with Zeneca. It is a thymonucleotide synthase inhibitor, a derivative of folic acid, used in the treatment of patients with advanced colorectal cancer. It was launched in the UK for the first time in 1996 under the trade name Tomudex, and it was launched in France and other countries in the same year. As a first-line treatment drug for advanced colorectal cancer, it has the advantages of less toxic and side effects, convenient administration, and low price, and is in great demand in China. [0003] The structural formula of raltitrexed is as follows: [0004] [0005] There is a chiral carbon center in the structure of ralt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 柴雨柱许建良储雪原王足兵兰公剑王华萍徐丹朱春霞田舟山
Owner NANJING CHIA TAI TIANQING PHARMA
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