الفهرس 
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Abstract
Tne theoretical ba ckground for ’different spectrophootometric methods with special interest to the derivative spectrophotometry has been explained in chapter 11 and applied for the quantitation of sixteen pharmaceutical compounds (mentioned in chapter I), in single component doses (chapter Ill), two-component doses (chapter IV), three component doses (cnapter V).
In single component spectrophotometric analysis, six pharmaceutical compound, have been quantitavely estimated in different pharmaceutical preparations
like acepifylline suppositories} acetaminophen tablets and syrup, cinchocaine cream, oxyphenbutazone supposiitories, phenylbutazone tablets and saccharin tablets and syrup. Prior to such assays, the spectral characcteristics for the analysed compounds have been interrpreted and the optimum parameters for the quantitative assays were learned. The first derivative and the
second derivative methods were assessed and statistically compared with other spectrophotometric methods
(convential Amax/orthogonal function method). The
resul ts obtained are su.mrnarized in Table 34. from
these results the following conclusions can be outlined:
Drug
Amaxmethod
Recove-ry + C.V.
Dlmethod D2method
b)
O:f:f icial me.thod
Orthogonalli’uncti.on method
Aceplfylline
97~O’]+2 .• 03 CCT-97:10+1. 49~ t=0.03 2.2J* F=1.86 5.43* 98.26±1. 42 (c)
t=1.21 2.23* F=2.00 5.43*
98.04+1. 03 (b)
- JE
t= 1.86 2.31
F= 4.20 6.39]E
102.90+0.61 (b )10J.24+0. 53 (b)
t = o. 55 - 2 • 3 1 * t == 0-. 91- 2 _. 3l i F= 1.85 6.39* F= 1.JO 6.J9JE 258.09+15.04(c)137.38+1•64(c) 135.54: 4.49(c)103.05+1•06(c)
97.03* 0.65(d) 96.62+1.14(d) t= 0.86 2.18*
F= 3.D9 4.28JE
Acetaoinophen {b)
a- Tablets 97.10+0.51
(500mg) -
I--’ ()\ \..0
b- Syrup 103.16+0.8J(b)
(120mg/5m1) -
Cinchocaine cre am (l:;m ’&)
Oxyphenbutaazone E;UPPOOsitor1e8
(100 mg)
(w1 th respect to D2 )
102.90+0.55(a) ( ::anufacture
- method ) Pheny1buta- 97 ~ 49+ -0’:43 (C)96~-48~O: 76 re)
zone tablets - JE
( 200 mg ) t= 2.93 2.23
F= 3-.00 5.43JE
Drug
Sacchorin sodium
a- Syrup
b- Tablets
A maxmethod
~ Recovery ~ c. V~ (%)
Dlmethod D2method
Official method
Orthogonallfunction method
,
(e) (e)
103-. 72±1-.45 101.70+1.10
JE t= 3. 3, 2.” 10
F= 1.8 3.26*
100.44.±O.93(b) t= 2.16 2016*
*
F= 3.26 6,00 ~
(with resp~ct ~
to Dl ) (lJ
102. 66.±L 56 (a) -I
10S.20±1.J6(e)100.72±0.92(e) before filt- t= 8.3 2.1 JE
ration ~= 2.39 3.2 *
102.40±1.26(e 101040+1.71(e)
after filt- t=1.46 2.1 JE
ratiQn F=1.80 3.2 JE (a)-, Cb), (c), (e) are HO of experiments which equal (3), (5), (6), (7), (10).
- C.V~= Cnefficient of variation •
. - The staTred figures are the corresponding theoretical values for F & t.
- The figures: in parenthesis are the assay values of laboratory made mixtures.
- F and t value8 calculated with respect to A method.
max
. Although the derivativ6 spectrophotomet~ic method can be applied to wide range of concentration, yet it is of comparable sensitivity, witp Amax and other methods •
. The accuracy of derivative spectroph~tomGtry method is comparoble to the Amax method providing that,
a) the compound to be determined exhibites h~gh abworbance coefficient, b) the compound exists
in large dose. The high dilution necessary, there~ fore, for -Amax and Dl measurement minimizes the irrelevant a~sorbance contribution to such a degree thst nullifies its effect on the results of A
max
method. In small doses however and where the
excepient is also minor like saccharin tablets, derivative spectrophotometric• method gives more accurate results compared with convential absorpption (Amax) method. Moreover, use of derivative spectrophotometry may preclude filtration process prior to absorbance measurement, and thereby ~ender t~e procedure simpler and faster.
3, The derivative spectrum is always having at least two Dl~optimum values, one cQrrespond~ng to the positive slope anQ the other to the negative slope
. Although the derivativ6 spectrophotomet~ic method can be applied to wide range of concentration, yet it is of comparable sensitivity, witp Amax and other methods •
. The accuracy of derivative spectroph~tomGtry method is comparoble to the Amax method providing that,
a) the compound to be determined exhibites h~gh abworbance coefficient, b) the compound exists
in large dose. The high dilution necessary, there~ fore, for -Amax and Dl measurement minimizes the irrelevant a~sorbance contribution to such a degree thst nullifies its effect on the results of A
max
method. In small doses however and where the
excepient is also minor like saccharin tablets, derivative spectrophotometric• method gives more accurate results compared with convential absorpption (Amax) method. Moreover, use of derivative spectrophotometry may preclude filtration process prior to absorbance measurement, and thereby ~ender t~e procedure simpler and faster.
3, The derivative spectrum is always having at least two Dl~optimum values, one cQrrespond~ng to the positive slope anQ the other to the negative slope
Table 35e; Assay Results of Assaying One Component in Presen~e ef coexisting . component (s) •.Component to be analysed Coexisting 1st
X% Recovery + C.V.(%) .
Component (s) ----.~-:_---_ ..
2nd Amax- method Dl- method 155.54±0.37 100.46±0.72
t = 205.058 2.075~
F = 1.560 2.760~
(124.70t7142)(100.72±0.55)
1. Acepifyllin’€~ 4 parts in 8up)o8ito~i€s
204.36±1.26 t = 94.24 F = 6.75 (98.83j),,97) t = 0.02 F = 6.70
Phenobarbiitone,l part
2. Procaine .HCl, 10 parts inalllp onl e s
Caffeine anhyydrous, 7parts
t = 8 .• IS F = 282.47
=98.14±1.01 2.23~
5.34*
(98.85±O.76) 2.23]£
5.34]£
I f--’ (/’1 0’
~
2.11~ 3.21* the problems of assaying single component jn mQlti~ component mixtures. In other words the method can correct for the irrelevant absorbance due to the exoepient in the pharmaceutical preparatio~s as well as absorption of coexisting compon8nts, if any.
In simultaneous two-component analysis, four two-component mixtur~s have been quantitated and the results are summarized in Table 36. The results of
the derivative spectrophotometry have been stHtistically compared with Vierordt’s method. In some pharmaceutical preparations where the irrelevant absorbance contripu~ tion due to excepient is significant, Vierordt’s method gives inaccurate results, e.g. procaine-caffeine ampoul~s, acepifylline-phenobarbitone suppositories. More important, the limitations for Vierordt’s method application (page 11 , ’\2 ) are not necessary when
we are dealing with the ut~lity of derivative spectroophotometric method. Meanwhile, unlike Vierordt’s method, the derivative spectrophotometric method can pe used for simultaneous determination of minor and major component with the s8me accuracy and precision.
Two three component mixtures have be~.p. anqlysed using three simultaneous equations. The results
obtained are summarized in Toble 37.
It shou:Ld be
emphasized that the simultaneous assays of three cemponents mixtures have been poorly approached in the c~rrent literature and all the quantitative methods depen- on the prior separation of different components. The results obtained via Amax value measurements are unacceptable as they are neither
accurate nor precise.
Good results however have
been obtained on applyin~ Dl three-component method. It is therefore expectable that, the utility of this method in such type of analysis will defintly enrich the future literature.