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Method for separating and detecting gatecarboxylic acid ethyl ester and/or related impurities by HPLC (High Performance Liquid Chromatography) method

A technology for the addition of ethyl carboxylate and ethyl carboxylate, which is used in material separation, measurement devices, analysis materials, etc., to achieve the effects of strong specificity, good reproducibility and high sensitivity

Pending Publication Date: 2022-03-01
CHONGQING HUABANGSHENGKAI PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] At present, there is no relevant literature or data to disclose the method for separating the above-mentioned gaticarboxylate and 9 impurities and measuring the content of 7 impurities

Method used

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  • Method for separating and detecting gatecarboxylic acid ethyl ester and/or related impurities by HPLC (High Performance Liquid Chromatography) method
  • Method for separating and detecting gatecarboxylic acid ethyl ester and/or related impurities by HPLC (High Performance Liquid Chromatography) method
  • Method for separating and detecting gatecarboxylic acid ethyl ester and/or related impurities by HPLC (High Performance Liquid Chromatography) method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] Take an appropriate amount of this product, accurately weighed, add diluent [water-acetonitrile (1:1)] to dissolve and quantitatively dilute to make a solution containing about 1mg in every 1ml, as the test solution (put it into the control immediately after preparation) 5°C sample tray); accurately measure 5.0ml, put it in a 50ml measuring bottle, dilute to the mark with diluent, shake well, then precisely measure 2.0ml, put it in a 100ml measuring bottle, dilute to the mark with diluent, Shake well as a control solution. Use octadecyl bonded silica gel as filler (4.6mm×250mm, 5μm); use buffer salt (weigh 2.0g potassium hexafluorophosphate, add 1000ml water to dissolve, add 3.0ml triethylamine, adjust pH 3.0 with phosphoric acid) Be mobile phase A, with acetonitrile as mobile phase B, carry out linear gradient elution according to Table 1, detection wavelength is respectively 250nm and 220nm (the measurement wavelength of impurity MOXH-SM1e is 220nm, and the detection ...

Embodiment 2

[0074] Exclusive

[0075] Impurities that may exist in SM1: Impurity MOXH-SM1a, Impurity MOXH-SM1b, Impurity MOXH-SM1e, Impurity MOXH-SM1m, Impurity MOXH-SM1g, Impurity MOXH-SM1h, Impurity MOXH-SM1j, Impurity MOXH-SM1f, Impurity MOXH- SM1i has a total of 9 impurities. In this method, a total of 7 impurities of impurity MOXH-SM1a, impurity MOXH-SM1b, impurity MOXH-SM1e, impurity MOXH-SM1m, impurity MOXH-SM1g, impurity MOXH-SM1h, and impurity MOXH-SM1j will be carried out. Research. Take 10 μl each of the blank solution, each impurity positioning solution, the test solution, and the mixed solution respectively, inject samples in sequence, and record the chromatogram. The measurement results are shown in Table 2-4, attached Figure 1-2 .

[0076] Table 2 Specific 250nm HPLC chromatogram integration results

[0077]

[0078] Table 3 Specific 220nm HPLC chromatogram integration results

[0079]

[0080]

[0081] Table 4 specificity test results

[0082]

[0083] Co...

Embodiment 3

[0085] detection limit

[0086] The detection limit solution was taken for three consecutive injections, and the ratio of the main peak height to noise (signal-to-noise ratio) was calculated. The test results are shown in Table 5-7, attached Figure 3-4 .

[0087] Table 5 Detection limit 250nm HPLC chromatogram

[0088]

[0089] Table 6 Detection limit 220nm HPLC chromatogram integration result

[0090]

[0091] Table 7 Detection limit determination result

[0092]

[0093]

[0094] Conclusion: The detection limit concentration of impurity MOXH-SM1e is 0.069 μg / ml, which is expressed as 0.007% by the concentration in the sample, and the average signal-to-noise ratio is 3.8; the detection limit concentration of impurity MOXH-SM1g is 0.067 μg / ml, which is expressed by the concentration in the sample Expressed as 0.007%, the average signal-to-noise ratio is 11.2; the detection limit concentration of impurity MOXH-SM1b is 0.073 μg / ml, expressed as 0.007% in the con...

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Abstract

The invention relates to the technical field of pharmaceutical analysis, in particular to a method for analyzing ethyl gatetanecarboxylate and related impurities by using high performance liquid chromatography. A chromatographic column adopted by the method takes octadecyl bonded silica gel as a filling agent, a buffer salt solution and an organic solvent are adopted for gradient elution, the flow velocity is 0.9-1.1 ml / min, and the column temperature is 18-22 DEG C; the detection wavelength is 220 nm or 250 nm; the method can effectively separate and accurately quantify seven known impurities possibly existing in the starting material ethyl gatetanecarboxylate of moxifloxacin hydrochloride within 42 minutes, the separation effect of the other two known impurities possibly existing in the starting material and the seven known impurities is good, and the method has no interference on impurity identification and quantitative detection. The problem of separation and determination of known impurities in ethyl gatetanecarboxylate, which cannot be solved in the prior art, is provided; the analysis method is high in sensitivity; the specificity is high; the reproducibility is good; the operation is simple and feasible.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a method for analyzing ethyl gaticarboxylate and related impurities by using high-performance liquid chromatography. Background technique [0002] Moxifloxacin is an almost white crystalline powder chemical with the formula C 21 h 24 FN 3 o 4 , fluoroquinolone antibiotics. DNA topoisomerase inhibitors can be used to treat socially acquired pneumonia caused by Staphylococcus aureus, influenza bacillus, pneumococcus, etc., acute exacerbation of chronic bronchitis, acute sinusitis, etc. It belongs to the fourth generation of quinolone antibacterial drugs and is a new generation of antibiotics with a broad antibacterial spectrum. This product has strong antibacterial activity against common respiratory bacteria, such as Streptococcus pneumoniae, Haemophilus influenzae, Morahan catarrhalis and some Staphylococcus aureus. Especially for Streptococcus pneumoniae, it has a str...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/34G01N30/32G01N30/30G01N30/06G01N30/74G01N30/88G01N30/86
CPCG01N30/02G01N30/34G01N30/32G01N30/30G01N30/06G01N30/74G01N30/88G01N30/8634G01N2030/324G01N2030/8872G01N2030/884Y02P20/55
Inventor 张荣周春燕
Owner CHONGQING HUABANGSHENGKAI PHARM
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