Method for simultaneously detecting various gene impurities of vilanterol triphenylacetate

A technology for vilanterol triphenylacetate and impurities, which is applied in the field of analytical chemistry, can solve the problems of high sensitivity requirements of detection methods, difficult quantitative detection, and difficult separation, achieves a good linear relationship, ensures product quality, and has high sensitivity. Effect

Pending Publication Date: 2022-05-06
SHANGHAI FANGYU HEALTH PHARMA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is precisely because of its low content limit and high sensitivity requirements for detection methods that it is difficult to achieve quantitative detection
Moreover, the polarities of the three impurities are relatively close, and the separation is difficult
At present, there is no literature report on the simultaneous qualitative and quantitative detection of these three potential genotoxic impurities

Method used

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  • Method for simultaneously detecting various gene impurities of vilanterol triphenylacetate
  • Method for simultaneously detecting various gene impurities of vilanterol triphenylacetate
  • Method for simultaneously detecting various gene impurities of vilanterol triphenylacetate

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0099] Preparation of test solution I: Weigh 305.52 mg of vilanterol triphenylacetate raw material, put it in a 10ml measuring bottle, add 60 μl of VL02imp4, VL02imp6, VL02imp8 positioning solution respectively, add methanol to dilute to the mark, shake well, Instantly. (Preparation of localization solution: Weigh 5.24mg of VL02imp4, accurately add 1ml of methanol to dissolve, and then obtain VL02imp4 localization solution. Prepare VL02imp6 and VL02imp8 localization solutions in the same way, and weigh 5.54mg and 5.78mg respectively.)

[0100] Measure need testing solution I with described chromatographic condition 1, record chromatogram, see figure 1 . figure 1 It is shown that the VL02imp8 and triphenylacetic acid chromatographic peaks cannot be baseline separated.

[0101] On the basis of chromatographic condition 1, the screening of chromatographic columns was carried out. Replace the capillary chromatographic column (DB-WAX, 0.32mm×30m, 0.5μm) with polyethylene glycol ...

Embodiment 1

[0121] Embodiment 1 Methodological verification of the detection method established by the present invention

[0122] 1.1 Specificity and system adaptability

[0123] Solution preparation:

[0124] (1) Blank solution: Take methanol (chromatographically pure) to get it.

[0125] (2) Test solution: Weigh 30 mg of vilanterol triphenylacetic acid (batch number: VL1709903, source: Livzon Synthetic Pharmaceutical Co., Ltd.), weigh it accurately, put it in a sample injection vial, add 1 ml of methanol to dissolve, and shake well , that is.

[0126] (3) Mixed reference substance stock solution: Take 15 mg each of VL02imp4, VL02imp6 and VL02imp8 reference substances, weigh them accurately, put them in the same 50ml measuring bottle, dissolve them with methanol and dilute to the mark to obtain the product. See Table 1 for the sample weight of each impurity reference substance.

[0127] Table 1 The weighing amount of three impurity reference substances

[0128] Impurity re...

Embodiment 2

[0180] Example 2 Determination of genotoxic impurities in different batches of vilanterol triphenylacetic acid

[0181] Chromatographic conditions:

[0182] Preparation of the test solution: Weigh 30 mg of vilanterol triphenylacetic acid, accurately weigh it (see Table 12 for the specific weighing amount), put it in a sample injection vial, add 1 ml of methanol to dissolve, shake well, and obtain.

[0183] Table 12 Vilanterol triphenylacetic acid sample volume records

[0184] batch number VL1709901 VL1709902 VL1709903 Sample weight (mg) 29.91 31.41 31.87

[0185] Preparation of reference substance solution: Weigh 14.34mg of VL02imp6 reference substance in a 50ml measuring bottle, dilute to the mark with methanol, and shake well; accurately measure 2ml in a 20ml measuring bottle, dilute to the mark with methanol, shake well, that is have to.

[0186] Determination: Accurately draw 1 μl each of the reference substance solution and the test solutio...

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Abstract

The invention discloses a method for detecting a genotoxic impurity containing bromohexyl in vilanterol triphenylacetate. The genotoxic impurity is selected from VL02imp4 of a structural formula I, VL02imp6 of a structural formula II and/or VL02imp8 of a structural formula III. The method is based on a gas chromatography-flame ionization detector, and the chromatographic conditions are as follows: 5% diphenyl-95% dimethyl polysiloxane is used as a capillary chromatographic column of a stationary liquid; the initial temperature is 35-45 DEG C, the temperature is increased to 315-325 DEG C at the speed of 13-18 DEG C/min, and the temperature is maintained The carrier gas is nitrogen, the flow velocity is 0.8-1.2 ml/min, the constant flow mode is adopted, and the split ratio is (8: 1)-(12: 1); the sample introduction temperature is 250 DEG C; the sample size is 1 microliter; the detection temperature is 315-325 DEG C, the flow rate of nitrogen is 25ml/min, the flow rate of hydrogen is 40ml/min, and the flow rate of air is 400ml/min.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for simultaneously detecting multiple gene impurities of vilanterol triphenylacetic acid. Background technique [0002] Vilanterol trifenatate, CAS#503070-58-4, the structural formula is shown in 1. [0003] [0004] Vilanterol triphenylacetate is a new long-acting β2-receptor agonist. Compared with other β2 receptor agonists, the compound has the advantages of faster onset of action, longer duration of action, higher selectivity, and better safety and tolerability in patients with asthma and COPD. Vilanterol can be combined with inhaled corticosteroids and anticholinergic drugs to form a compound or triple preparation for the maintenance treatment of asthma or chronic obstructive pulmonary disease (COPD). Products already on the market include umeclidinium bromide vilanterol inhalation powder (trade name: Orexin), fluticasone furoate vilanterol inhal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/68
CPCG01N30/02G01N30/68G01N2030/047
Inventor 夏晶王琦琦袁梦莹
Owner SHANGHAI FANGYU HEALTH PHARMA TECH CO LTD
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