药典流动相药大生药学0922e.pdfVIP

KetoprofenEUROPEANPHARMACOPOEIA7.0

Mobilephase:

—mobilephaseA:acetonitrileR1,3.4g/Lsolutionof

tetrabutylammoniumhydrogensulfateR(5:95V/V);

—mobilephaseB:acetonitrileR1,3.4g/Lsolutionof

tetrabutylammoniumhydrogensulfateR(50:50V/V);B.1-acetyl-4-[4-[[(2RS,4SR)-2-(2,4-dichlorophenyl)-2-(1H-

TimeMobilephaseAMobilephaseBimidazol-1-ylmethyl)-1,3-dioxolan-4-yl]methoxy]-3-[4-(4-

(min)(percentV/V)(percentV/V)acetylpiperazin-1-yl)phenoxy]phenyl]piperazine,

0-10100→00→100

10-150100

Flowrate:2mL/min.

Detection:spectrophotometerat220nm.

Equilibration:withacetonitrileRforatleast30minandthen

withmobilephaseAforatleast5min.C.1-acetyl-4-[4-[[(2RS,4RS)-2-(2,4-dichlorophenyl)-2-(1H-

imidazol-1-ylmethyl)-1,3-dioxolan-4-yl]methoxy]phenyl]-

Injection:10μL;injectmethanolRasablank.

piperazine,

Retentiontime:ketoconazole=about6min;loperamide=about

8min.

Systemsuitability:referencesolution(a):

—resolution:minimum15betweenthepeaksduetoD.1-[4-[[(2RS,4SR)-2-(2,4-dichlorophenyl)-2-(1H-imidazol-1-

ketoconazoleandloperamide;ifnecessary,adjustthefinalylmethyl)-1,3-dioxolan-4-yl]methoxy]phenyl]piperazine,

concentrationofacetonitrileinthemobilephaseoradjust

thetimeprogrammeforthelineargradientelution.

Limits:

—total:notmorethantheareaoftheprincipalpea