Separation and detection method for anticoagulant drugs
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A technology of polysaccharide derivatives and rivaroxaban, applied in the field of analytical chemistry, can solve problems such as separation and detection methods of undetected enantiomers
Active Publication Date: 2015-03-18
SUNSHINE LAKE PHARM CO LTD
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[0006] Quality control is required during the production of (S)-rivaroxaban, but currently, (S)-rivaroxaban is not recorded in the USP of the United States Pharmacopoeia, EP of the European Pharmacopoeia and Ch.P. of the Chinese Pharmacopoeia Shaban, also did not find the separation and detection method of (S)-rivaroxaban and its enantiomer reported in the literature
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Embodiment 1-4
[0057] Example 1-4: Method for separating and detecting (S)-rivaroxaban and its enantiomers with CHIRALPAK AS-H chiral chromatography column
[0065] Mobile phase: n-hexane (containing 0.1% diethylamine): ethanol (V / V) is 30:70 as the mobile phase;
[0066] Running time: 42min;
[0067] Experimental procedure
[0068] Release agent: acetonitrile:ethanol=60:40 (V / V); take about 25mg of rivaroxaban racemate, accurately weigh it into a 50mL brown measuring bottle, dissolve it with diluent and dilute to the mark, shake well, and use as Test solution. Get diluent (as blank solution) and need testing solution respectively, carry out high performance liquid chromatography analysis by above-mentioned conditions, record chromatogram, the result sees figure 1 , figure 2 . figure 2 The chromatographic peak with retention time of 17.000 ...
Embodiment 2
[0070] Take about 25mg of (S)-rivaroxaban (crude drug), accurately weigh it into a 50ml brown volumetric flask, dissolve it ultrasonically with a diluent and dilute to the mark, shake well, and use it as the test solution. Get need testing solution, carry out high performance liquid chromatography analysis according to the condition of example 1, record chromatogram, the results are shown in image 3 , wherein, the retention time is 33.640 minutes for (R)-rivaroxaban, 16.100 minutes for (S)-rivaroxaban. image 3 It is proved that the optical purity of (S)-rivaroxaban (crude drug) reaches above 99.4%, and this method can be used for quality monitoring of (S)-rivaroxaban raw material drug.
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Abstract
The invention belongs to the field of analytical chemistry and particularly relates to a method of separating and testing (S)-Rivaroxaban and enantiomers thereof by liquid chromatography. The method for separating and testing (S)-Rivaroxaban and enantiomers (impurities) thereof by liquid chromatography is characterized in that a polysaccharide derivative is used as a chiral chromatographic column of filler and a mixed solution of low alcohol or low alkane or low alcohol is used as a moving phase. According to the separation and detection method provided by the invention, (S)-Rivaroxaban can be effectively separated from enantiomers thereof, wherein the separation degree reaches over 1.5 and complete baseline separation is achieved, so that the quality of (S)-Rivaroxaban can be accurately and effectively controlled. The separation method provided by the invention can be used for separating and detecting the (S)-Rivaroxaban and enantiomers thereof within 80 minutes. The method provided by the invention can be used for simply, quickly and accurately separating and detecting (S)-Rivaroxaban and optical isomers thereof.
Description
technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for separating and measuring (S)-rivaroxaban and its enantiomers by liquid chromatography. Background technique [0002] PCT application WO2001047919 discloses rivaroxaban or its pharmaceutically acceptable salt for the first time, rivaroxaban, chemical name is 5-chloro-N-(((5S)-2-oxo-3-(4-(3- Oxomorpholin-4-yl)phenyl)-1,3-oxazolin-5-yl)methyl)thiophene-2-carboxamide, its chemical structure is as shown in formula (I), hereinafter referred to as (S )-rivaroxaban, [0003] [0004] (S)-rivaroxaban can competitively inhibit free and bound factor Xa and prothrombin activity, and prolong activated partial thromboplastin time (PT) and prothrombin time (aPTT) in a dose-dependent manner, mainly For the prevention of venous thrombosis (VTE) in adult patients undergoing elective hip or knee replacement surgery. In the United States, it is used to prevent the formation of ...
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