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Method for separating benzaldehyde and nitrobenzaldehyde by employing high performance liquid chromatography

A technology of high performance liquid chromatography and nitrobenzaldehyde, which is applied in the direction of material separation, analysis of materials, and measuring devices, to achieve good accuracy, good peak shape, and strong specificity

Active Publication Date: 2019-05-10
HINYE PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In order to solve the problem that existing analytical methods cannot separate and quantify benzaldehyde and o-, m-, and p-nitrobenzaldehyde simultaneously, the present invention provides a new method for separating and quantifying benzaldehyde and nitrobenzaldehyde

Method used

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  • Method for separating benzaldehyde and nitrobenzaldehyde by employing high performance liquid chromatography
  • Method for separating benzaldehyde and nitrobenzaldehyde by employing high performance liquid chromatography
  • Method for separating benzaldehyde and nitrobenzaldehyde by employing high performance liquid chromatography

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Embodiment 1: HPLC detection of lercanidipine hydrochloride bulk drug.

[0035] Instrument: Waters e2695-2489 high performance liquid chromatography

[0036] Chromatographic column: Phenomenes ACE Excel 5 C 18 -PFP (250*4.6mm, 5μm)

[0037] Mobile phase: 0.05mol / L dipotassium hydrogen phosphate (add 3ml of triethylamine, adjust the pH to 7.5 with phosphoric acid)-methanol (80:20)

[0038] Diluent: mobile phase

[0039] Detection wavelength: 240nm

[0040] Stationary phase temperature: 40°C

[0041] Flow rate: 1.0ml / min

[0042] Injection volume: 20μl

[0043] Workstation: Empower

[0044] Get 1.0g of lercanidipine hydrochloride bulk drug and add appropriate amount of mobile phase to dissolve and dilute to make lercanidipine hydrochloride 40mg / ml as need testing solution, get benzaldehyde, 2-nitrobenzaldehyde, 3-nitrobenzaldehyde in addition and 4-nitrobenzaldehyde reference substance in appropriate amounts, accurately weighed, added mobile phase to dissolve and...

Embodiment 2

[0047] Embodiment 2: Use this method to examine benzaldehyde and nitrobenzaldehyde in lercanidipine hydrochloride at different flow rates.

[0048] Instruments and reagents are the same as in Example 1, and other chromatographic conditions are the same as in Example 1 except for the flow rate. The flow rates for this study were 0.9 ml / min, 1.0 ml / min and 1.1 ml / min.

[0049] Take 2.0g of lercanidipine hydrochloride crude drug, add benzaldehyde, 2-nitrobenzaldehyde, 3-nitrobenzaldehyde and 4-nitrobenzaldehyde reference substance mother liquor, add appropriate amount of mobile phase to dissolve and dilute to make hydrochloric acid 40 mg / ml of lercanidipine, 3 μg / ml of benzaldehyde and 3 μg / ml of ortho-p-nitrobenzaldehyde plus impurities for the test solution. Take another appropriate amount of benzaldehyde, 2-nitrobenzaldehyde, 3-nitrobenzaldehyde and 4-nitrobenzaldehyde reference substances, weigh them accurately, add mobile phase to dissolve and quantitatively dilute to form ...

Embodiment 3

[0052] Embodiment 3: Use this method to check benzaldehyde and nitrobenzaldehyde in lercanidipine hydrochloride at different column temperatures.

[0053] Instrument and reagent are the same as Example 1, and other chromatographic conditions are the same as Example 1 except column temperature. In this study, the column temperatures were 38°C, 40°C and 42°C.

[0054] Solution preparation is the same as embodiment 2.

[0055] Take the blank solution (mobile phase), the mixed impurity reference substance solution, and the impurity-added lercanidipine hydrochloride test solution, measure according to the above chromatographic conditions, and record the chromatogram.

[0056] Test results: Calculated by the external standard method, within the column temperature range of 38°C to 42°C, the RSD% value of benzaldehyde content is 4, the RSD% value of o-nitrobenzaldehyde content is 1.4, and the content of m-nitrobenzaldehyde The RSD% value was 0.7, and the RSD% value of p-nitrobenzald...

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Abstract

The invention discloses a detection method for separating isomers of benzaldehyde and nitrobenzaldehyde by employing high performance liquid chromatography. The method includes steps: C-18 and 5-fluoropheny hybrid bonded silica gel is regarded as a stationary phase, dipotassium phosphate-methanol-organic aqueous alkali is regarded as a mobile phase, and an HPLC spectrogram is recorded with the detection wavelength of less than 240 nm. By employing the method, miscellaneous peak interferences with peak-outlet positions of benzaldehyde, o-nitrobenzaldehyde, m-nitrobenzaldehyde and p-nitrobenzoicacid reference substances can be eliminated, the specificity and the separation degree are superior to those of the conventional method, the durability is good, quality control can be better realized, and the pharmaceutical security is facilitated.

Description

technical field [0001] The present invention relates to the technical field of chemical drug analysis, in particular to a method for separating benzaldehyde and nitrobenzaldehyde (including ortho, meta and para isomers) using high performance liquid chromatography, and in particular to the detection of the chemical drug Lexyl Hydrochloride The possible impurity benzaldehyde and nitrobenzaldehyde (including ortho, meta and para isomers) in cardipine. Background technique [0002] Benzaldehyde and nitrobenzaldehyde (including ortho, meta and para isomers) are potential genotoxic impurities that may be introduced during the synthesis of chemical drugs. [0003] Genotoxic impurities refer to compounds that directly or indirectly damage cellular DNA, produce gene mutations or in vivo mutagenesis, and have the possibility or tendency to cause cancer. Potentially genotoxic impurities refer to structurally similar genotoxic impurities, which are warning, but have not been proved by...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 谢冰洁常玉良程雪清高玉贺宋志林
Owner HINYE PHARM CO LTD
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