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RESULTS
CZE
S eparatio n o f 4 TCA and pheno tia zine s tandards : dez ypramine (DEZ), no rtrytpyline (NOR), c hlo rproma zine (CHPRO) and pro ma zine (PRO)
0,007 0,006
MECC
Tablet e xtrac t of anafranil (c lo mipramine ) with inte rnal s ta ndard dox e pine (DOX)
0,0 03
NOR
DOX (IS )
0,005
0,004
0,00 25
CLO EOF
A [AU]
0,003
A [AU]
0,002
DEZ
PRO M
CHPRO E OF
0,0 02
0,001
0,00 15
0 0 -0,001 2 4 6 8 10 12 14
S ample
Se paratio n buffe r: 40 mM s odium te tra borate , pH 9,5 with a ddition 10 mM STDC.
0 5 10 15 20 25 30
Analyte
-0,002
0,0 01
t [min]
Blood Ta blet
Separatio n o f 5 TCA s tandards : no rtry ptyline (NOR), amitryptyline , (AMI), do xe pine (DOX), dezypramine (DEZ) and imipramine (IMI)
0,006
0,00 05
t [min]
AMI
0,005
0,004
NOR DOX EO F
0,003
A [AU]
0,002
DEZ
IMI
S epa ratio n o f drug mixture : amitry ptyline (AMI), c lomipramine (CLO), do xe pine (DOX) and imipra mine (IMI)
0, 006
0,001
0
-0,001
10
12
14
EOF
0, 005
AMI
0, 004
CONCLUSIONS
CLO S e paratio n buffe r: 40 mM s odium te tra bora te , pH 9,5 with a ddition 10 mM S TDC.
-0,002
t [min]
S e paration o f de zipram ine (DEZ), no rtryptyline (NOR), c hlo rpro m azine (CHPROM) and pro maznine (PROM) in the e xtrac t of blo o d
0, 012
A [AU]
0, 003
DOX
Both CZE and MECC may be used for identification of pharmaceutical preparations.
0, 002
IMI
0 ,01
NOR
0, 008 E OF
Extra ct of blood with drug mixture and IS (NOR) Extra ct of blood with IS (NOR)
The results of CZE blood analysis (spiked with drug standards) show that some drugs may be well separated (e.g.. desipramine, nortriptyline) while the others (e.g.. promazine, chlorpromazine) are not completely resolved from endogenous compounds of blood matrix. However, promazine is resolved enough to be determined in whole blood samples using standard addition method.
0, 001
0 0 5 10 15 20 25 30 35 40
A [AU]
0, 006 NOR 0, 004 CHP ROM P ROM 0, 002 DEZ 0 0 -0, 002 2 4 6 8 10 12 14 EOF
t [min]
S e paratio n Buffer: 50mM CAPS O in 30% v/v me tha nol; pH 9,5
The initial examinations on application of MECC to the separation of four TCA showed that using this mode, the protein fraction of blood matrix does not interfere with the examined drugs, however the peaks on electropherograms were broader and their relative times were less repeatable compared to those in the CZE
t [min]
De z ypramine (DEZ) - table t (Pe tylyl) e xtract with interna l s tandrad additio n o f imipramine (IMI)
0,01
CLO
0,0 08
0,0 06
mode. The further examinations in this matter should be carried out. Generally, it may be concluded that for the air thermostated capillary electrophoresis system, CZE mode seems to be preferable rather than MECC, especially in the cases of multi-drug analyses (e.g. screening analyses). However cleaner blood extracts (e.g. using SPE technique) are required. The alternative way for the improvement of the extraction process might be the application of the combined CE modes, for example CZE with addition of appropriate amount of surfactant.
DE Z
0,006
A [AU]
0,008
0,0 04
A [AU]
IMI (IS)
0,004
0,0 02
EOF
0
0,002
EOF
10
0 0 2 4 6 8 10 12 14
-0,0 02
t [min]
-0,002
t [min]