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Bilastine detection method

A detection method and a bilastine technology, which are applied in the field of analytical chemistry, can solve the problems that bilastine does not affect the efficacy of bilastine raw materials and its preparations, and achieve the effect of improving accuracy.

Inactive Publication Date: 2015-06-24
BEIJING COLLAB PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, because bilastine is not very stable, the drug itself is prone to degradation during the placement process, and some by-product impurities are easily introduced during the preparation process. These impurities are all related substances of bilastine, which will affect Therefore, for the impurities introduced in the synthesis route and the impurities introduced in the degradation of bilastine, strict inspections must be carried out in the bilastine raw material and its preparations. Therefore, effective detection of all potential impurities of bilastine is of great significance in the process improvement of bilastine synthesis process, the quality control of raw materials and the quality control of preparation products

Method used

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Experimental program
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Embodiment 1

[0039] Sample preparation

[0040] Take bilastine, formula (II), formula (III), formula (IV), formula (V), formula (VI), formula (VII) and bilastine oxidation damage samples respectively, add acetonitrile and water volume Acetonitrile aqueous solution with a ratio of 50:50 was used to make a mixed solution containing about 0.06 mg / mL of bilastine and about 0.002 mg / mL of each impurity monomer, which was the sample to be tested.

[0041] Wherein, the bilastine damaged sample was obtained by mixing 20 mg of bilastine with 2 mL of 30% hydrogen peroxide and reacting at 50° C. for 30 minutes.

[0042] The oxidative damage sample solution and the mixed solution of other impurities are mixed again for chromatographic analysis, and the chromatographic analysis is carried out immediately for the sample to be tested. For the results, see figure 1 , figure 1 It is the HPLC collection of illustrative plates that according to the test method described in the embodiment of the present inv...

Embodiment 2

[0059] Sample preparation

[0060] Take the bilastine bulk drug and add acetonitrile and water with a volume ratio of 50:50 in an acetonitrile aqueous solution to make a solution containing about 2 mg / mL of bilastine, which is the sample to be tested.

[0061] The obtained sample to be tested is subjected to chromatographic analysis, and the results are shown in image 3 , image 3 It is the HPLC collection of illustrative plates that according to the test method described in the embodiment of the present invention 2, the sample to be tested described in the embodiment 2 is detected;

[0062] Instrument: Agilent 1100 (or 1200) high performance liquid chromatography and its workstation VWD (or DAD) detector

[0063] Chromatographic column: Agilent Eclipse XDB-C184.6×150mm, 5μm

[0064] Mobile phase A: 0.01mol / L ammonium acetate buffer (containing 0.1% triethylamine, 0.05% sodium heptanesulfonate, adjust pH to 5.0 with acetic acid)

[0065] Mobile Phase B: Acetonitrile

[0...

Embodiment 3

[0076] Sample preparation

[0077] Take an appropriate amount of bilastine preparation fine powder, approximately equivalent to 20mg of bilastine, put it in a 10mL measuring bottle, add an appropriate amount of acetonitrile aqueous solution (diluent) with a volume ratio of acetonitrile and water of 50:50 and sonicate for 15min, then add the diluent Dilute to the mark, shake well, filter, and take the filtrate as the sample to be tested.

[0078] Prepare the blank excipient solution in the same way to obtain the blank control sample.

[0079] The obtained sample to be tested is subjected to chromatographic analysis, and the results are shown in Figure 4 , Figure 4 For according to the test method described in the embodiment of the present invention 3 to the HPLC collection of illustrative plates of the sample to be tested described in embodiment 3;

[0080] The blank control sample was carried out chromatographic analysis, the results can be found in Figure 5 , Figure ...

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Abstract

The invention provides a Bilastine detection method. The Bilastine detection method comprises the steps of performing chromatographic analysis on a to-be-detected test of Bilastine, and obtaining each impurity in Bilastine, wherein a chromatographic analysis mobile phase is an inorganic salt buffer solution containing an ion pair reagent and an organic solvent. By adopting the inorganic salt buffer solution containing the ion pair reagent to serve as the chromatographic analysis mobile phase, the detection method can well separate each impurity in Bilastine and improve detection accuracy and can be used for quality monitoring of Bilastine raw material and preparations of the Bilastine raw material.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for detecting bilastine. Background technique [0002] Bilastine is a non-sedating, long-acting histamine antagonist that selectively antagonizes peripheral H1 receptors and can be used for the treatment of seasonal and perennial allergic rhinitis, conjunctivitis and urticaria. The chemical name of Bilastine is 2-[4-(2-(4-(1-(2-ethoxyethyl)benzimidazol-2-yl)piperidin-1-yl)ethyl)phenyl ]-2-methylpropionic acid, CAS No. 202189-78-4, molecular formula C 28 h 37 N 3 o 3 , the structural formula is shown in formula (I), [0003] [0004] However, because bilastine is not very stable, the drug itself is prone to degradation during the placement process, and some by-product impurities are easily introduced during the preparation process. These impurities are all related substances of bilastine, which will affect Therefore, for the impurities introduced in the synthe...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 张秋佳李瑞芳杨秋菊邹德超王珂赵大龙
Owner BEIJING COLLAB PHARMA
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