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Low-concentration retapamulin determination method and application

A technology of retamoline and determination method, which is applied in the directions of measuring devices, instruments, scientific instruments, etc., to achieve the effects of high sensitivity and accuracy, strong specificity and good repeatability

Active Publication Date: 2016-03-30
CHONGQING HUAPONT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] So far, no published method has been reported to be effective for the quantitative determination of low concentrations of retapamulin

Method used

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  • Low-concentration retapamulin determination method and application
  • Low-concentration retapamulin determination method and application
  • Low-concentration retapamulin determination method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Embodiment 1 Determination of retapamulin ointment transdermal test receiving liquid sample

[0058] Chromatographic conditions:

[0059] Chromatographic column: SHIMADZUVP-C18250×4.6mm, 5μm;

[0060] Mobile phase: methanol: 10mM ammonium acetate aqueous solution (75:25);

[0061] Mass spectrometry conditions: detection in positive ion mode; drying gas: N 2 ;Drying gas pressure (Gas2): 70psi; Ionization temperature (TEM) is 300°C; Atomization gas (Gas1) is 9psi; Curtain Gas (CurtainGas) is 12psi; Spray voltage (IonSprayVoltage) is 4700V; Collision gas (CAD) 6psi; injection voltage (EP) 10V; collision cell exit voltage (CXP) 20V;

[0062]

[0063] Detection method:

[0064] Standard curve and quality control: take retapamulin reference substance solution and tiamulin reference substance solution, respectively prepare 0.504ng / ml, 1.01ng / ml, 2.02ng / ml, 5.04ng / ml, 20.2ng / ml A series of solutions of , 40.3ng / ml and 60.5ng / ml are used as the standard curve, and the pe...

Embodiment 2

[0066] The determination of the intradermal sample of embodiment 2 retapamulin ointment transdermal test

[0067] Chromatographic conditions:

[0068] Chromatographic column: SHIMADZUVP-C18250×4.6mm, 5μm;

[0069] Mobile phase: methanol: 10mM ammonium acetate aqueous solution (75:25);

[0070] Mass spectrometry conditions: detection in positive ion mode; drying gas: N 2 ;Drying gas pressure (Gas2): 70psi; Ionization temperature (TEM) is 300°C; Atomization gas (Gas1) is 9psi; Curtain Gas (CurtainGas) is 12psi; Spray voltage (IonSprayVoltage) is 4700V; Collision gas (CAD) 6psi; injection voltage (EP) 10V; collision cell exit voltage (CXP) 20V;

[0071]

[0072] Detection method:

[0073] Standard curve and quality control: take retapamulin reference substance solution and tiamulin reference substance solution, respectively prepare a series of solutions of 101ng / ml, 126ng / ml, 151ng / ml, 176ng / ml and 202ng / ml as For the standard curve, the peak area is determined by injecti...

Embodiment 3

[0075] The determination of the sample on the skin of embodiment 3 retapamulin ointment transdermal test

[0076] Chromatographic conditions:

[0077] Chromatographic column: SHIMADZUVP-C18250×4.6mm, 5μm;

[0078] Mobile phase: methanol: 10mM ammonium acetate aqueous solution (75:25);

[0079] Mass spectrometry conditions: detection in positive ion mode; drying gas: N 2 ;Drying gas pressure (Gas2): 70psi; Ionization temperature (TEM) is 300°C; Atomization gas (Gas1) is 9psi; Curtain Gas (CurtainGas) is 12psi; Spray voltage (IonSprayVoltage) is 4700V; Collision gas (CAD) 6psi; injection voltage (EP) 10V; collision cell exit voltage (CXP) 20V;

[0080]

[0081] Detection method:

[0082] Standard curve and quality control: take retapamulin reference substance solution and tiamulin reference substance solution, respectively prepare a series of solutions of 161ng / ml, 181ng / ml, 202ng / ml, 222ng / ml and 242ng / ml as For the standard curve, the peak area is determined by injecti...

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Abstract

The invention belongs to the field of analytic chemistry and relates to a low-concentration retapamulin determination method and an application, in particular to a method for determining low-concentration retapamulin with high-performance liquid chromatography-tandem mass spectrometry as well as an application. According to the method, the high-performance liquid chromatography-tandem mass spectrometry is adopted for determination, the mass spectrum adopts a multi-reaction monitoring mode, further, an internal standard method is adopted, and tiamulin is taken as an internal standard substance. The determination method has the advantages of high specificity, sensitivity and accuracy and good repeatability, the limit of detection can be up to 200 pg / ml, the limit of quantitation can be up to 500 pg / ml, and the determination method can be widely applied to concentration tests of low-concentration retapamulin biological samples, especially sample concentration testing of retapamulin ointment transdermal tests, and has great significance for retapamulin quality control.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for measuring low-concentration retapamulin and its application. Background technique [0002] Retapamulin is a pleuromutilin semisynthetic antibiotic that can be used to treat impetigo and infections in small lacerations, abrasions, or sutured wounds. Molecular formula is C 30 h 47 NO 4 S, the chemical name is [[(3-external)-8-methyl-8-azabicyclo[3.2.1]octane]-3-mercapto]-, (3aS,4R,5S,6S,8R, 9R,9aR,10R)-4,6,9,10-Tetramethyl-5-hydroxy-6-vinyl decahydro-1-oxo-3a,9-propane-3aH-cyclopentacyclooctane-8 - Acetate, its chemical structural formula is as follows: [0003] [0004] It can be seen from the above structural formula that there is no conjugated group, the ultraviolet absorption is weak, and the maximum absorption wavelength is 209nm. At this wavelength, the baseline noise is large and there is much interference; The dosage is 10mg / skin slice, ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/8809
Inventor 颜波谭辉兰昌云张吉周维
Owner CHONGQING HUAPONT PHARMA
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