ANSWERS/ CLARIFICATIONS RAISED BY THE EXAMINER

Name of the Student : M.Vijaya Narasimha

Register . No. :0803PH0439
Title of the Thesis : Electrochemical and spectrophotometric studies of some medicinally
important drugs

Faculty : Chemistry
The detailed clarification for the questions raised by the examiner given below:
S.No. Question raised by the examiner Answer/Clarification
1. on page 5, line 12: mixed with in corrected as inactive (Pg.5)
active …" should read " …mixed
with an in active.
2. on page 6, it is stated that the basic The details are furnished (Pg.6)
principle of spectrophotometer is
absorbance of light; well, this is not
all what it is and there is much more
to it.
3. one page 48 (last line) - 49 (first and The sentence is revised and related literature is
second lines), it has been stated that cited and included in page.48-49. No contrary is
" a peculiar behaviour was observed mentioned in page.50.
that absent of anodic peak in reverse
scan and … due to the reduction of
azomethine group to saturated amine
derivation …"is there precedence for
this in the literature". And contrary to
what has been mentioned on age 50
(chapter 5)
4. "d.p.p. techniques have been applied DPP is an important analytical technique being
for the quantitative estimation of the used in quantitative estimation of drugs and
drug…"but no quantification has pharmaceutical formulations. In the present
been made. research work, the DPP technique is optimized
and the evaluated quantitative data was
furnished in the form of tables in chapter.5
(Pg.No:56,68,79). The quantification details
have been incorporated in appropriate places.
(Pg.No:50,61,72 ).
5. although IR spectra have been given, The sample medium was prepared with an oily
there is no mention of the medium in mulling agent (usually mineral oil called Nujol).
which the spectra have been A thin film of the mull is applied onto salt
recorded; also, none of the peaks plates and measured. The resultant spectral
have been assigned. peaks have been assigned specific values.
6. what are the error bars in the The values reported in Table 5.1, 5.4 and 5.7 are
polarographic (tables 5.1, 5.4, 5.7) experimental results and not analytical data ie
should be give only like correlation coefficient, standard deviations.
up to two significant digits and not Hence, error bars were not applied in the
three revised thesis.
7. identification of the reduced product Controlled potential electrolysis technique is
(page 60) is based solely on IR being used to reduce the electroactive
spectral data - thesis not convincing compound on mercury pool electrode whose
1

8. Scheme given in fig.5.20 (page 71) is
not clear, it should be redrawn. What
is the species formed in the first step?
How was the rate determining step in
this scheme established?
9. The textual material on page 72 are
all verbatim reproductions of textual
material from previous sections. this
should not be done
10. It is not clear as to how the diffusion
coefficient, transfer coefficient. rate
constant valued (page 73) were
obtained
11. All the figures (ir spectra, cvs and
polarographs) seen to have been
reproduced from author's published
papers. quality of reproduced figures
is very poor
12. In chapter 6, results of
spectrophotometric studies have been
described from all the spectral data,
instead of wt/vol. a better way to
express the concentration is molarity.
13. With regard to the accuracy of the
proposed method (table 6.3, page 86).
it is not clear as to how the value of
amount found, determined. And with
regard to robustness of the proposed
methods (table 6.4 (page 86)), has the
reproducibility check done? is the
method reproducible.
14. In table 6.10 (page 100), %
absorbance is given. absorbance is
just a number, it is not percentage .
15. In table 6.11 (page 100) a recovery of
101% (5th column, 1st row) has been
mentioned. How is it possible to
potential is kept constant by means of
potentiostat. The process of electrolysis is
continued till all the electro active species
disappears. When the electrolysis is completed a
second polarogram is recorded and found no
wave indicates the complete reduction of
electroactive functional group. This was
confirmed by IR spectral studies with respect to
the functional group ie azomethine to amine
group.
The scheme in Fig.5.20 (Pg.No: 71) is redrawn
and included in the thesis. Millicoulometry
technique was employed to determine total
number of electrons involved in the reduction
processes and on this basis, rate determining
step is established.
All verbatim reproductions of textual material is
revised and incorporated at relevant places.
On the basis of mathematical equations
(Eq.Nos:4,4.4,4.6,4.7,4.8.) mentioned in
chapter.4, the diffusion coefficient, transfer
coefficients, rate constant values evaluated.
All the voltammograms and IR spectra’s were
redrawn and incorporated in appropriate places.
Results of spectrophotometric studies were
expressed the concentration in molarity instead
of wt/vol in all the places of chapter.6
The accuracy of the proposed method was
established with the help of LOD,LOQ,
precision and standard addition methods. The
related mathematical formula is cited in chapter.
4 eq.Nos:4.9,4.10(page. No:44)The established
procedure is reproducible and it was checked
reproducibly.
It is corrected and incorporated in page. No:
100.
In the evaluation of percentage recovery, there
will be chance of dilution error or instrumental
error. In view of this, 101% of recovery
2
 recover more than what has been happened. As per quantification limits, the
started with? percentage of recovery will be 80-120 for
finished drugs.
16. It has been mentioned (page 102) that The context of mentioning of bio-availability
the methods used in this study would and pharmacokinetics profile of any drug in
provide bio-availability and blood, urine, and other biological fluids is that
pharmacokinetics profile of any drug Electro analytical and Spectrophotometric
in blood, urine, and other biological techniques were employed to explore the above.
fluids. Contrary to this statement. the But the aim of the present study is to optimize
present study did not include aspects the method of quantification of drugs using
pertaining to bio-availability so it Electroanalytical and spectrophotometric
cannot be claimed that this study will methods but not measurement of bio-
provide information about bio- availability of drugs in various biological fluids.
availability
17. On page 104 (2nd paragraph), no Comparative study of the research work carried
comparisons have actually been made out with different techniques in corporate in
with other techniques. table. 7.2.
18. Incorrect usage of articles "a" and All the mentioned usage of articles were
"an" : several instances article "an" corrected in the entire thesis.
has been used for consonants and
article "a" has been used for vowels.
This must be corrected everywhere in
the thesis (there are several of them).

19. Etcetra is etc and not e.c.t.: this need e.t.c has been corrected as etc in the appropriate
to be corrected in several places in places of the thesis.
the thesis.

20. Page 1. line 5 from bottom: " but In correct usage has been corrected in the thesis
whereas" - incorrect usage (two
negatives);either"but"or "whereas"
but not both together.

21. Page 2. table 1.1: "paracetamol" and Spellings were corrected in respect of
"salbutamol" mis-spelt. Paracetamol and Salbutamol

22. Page 3. line 3 from bottom: Misspell word is corrected.

"excreted" mis-spelt.

23. Page 5: pH-incorrect; correct The pH is corrected.

way:pH.

24. page 8. last para line: beer-lambers The Beer-Lambert’s word is corrected.
law should read " beer l ambert's law

25. correct usage of between: between 'x' The stated error is corrected in the entire thesis
and 'y' and not between 'x' to 'y' ; this wherever it appears.
must be corrected throughout the
thesis

3
26. Page 16, 2nd Para: poor sentence The sentence is refined.
framing; should be reframed to read
better.

27. page 16, line 8 from bottom; The misspell one is corrected as Stoichiometric
stoichiometric mis-spelt

28. Page 19, last Para: poor sentence The paragraph is revised and incorporated.
framing; should be reframed to read
better.

29. Page 25, 3rd Para: poor choice of The paragraph is revised and incorporated in
words, reframe to read better. page.No 25

30. page 32 , line 11 from bottom: faradic Misspell is corrected.

should read " faradaic"

31. Page 38. line 6: plateau mis-spelt Misspell is corrected

32. Page 40" "… where and the exposed The sentence is reframed.
…" problem with sentence framing.

33. Page 43, line 1: "beer law" should It is corrected as Beer-Lambert’s law and
read "beer lamberts law". incorporated in the thesis.

34. page 47, line 2: polar graphic should It is corrected as “polarographic” and included
read polarographic in the thesis.

35. Page 65, figure 5.16: label for y-axis The figure is redrawn and included in the thesis.
missing.

36. page 68, sub-heading of section 5.3: The spelling is corrected as chemical.
chemical mis-spelt

37. page 69, line 8: orthoshosphate mis- The spelling is corrected as “orthophosphate”
spelt

38. careful mis-spelt throughtout the The word is corrected as “careful”

thesis; it must be corrected

39. page 82, line 9 from bottom: The correct usage of word “ absorbance”
"absorbencies" - incorrect usage; included in the thesis.
correctusage "absorbance"
40. page 82 last but one line: replace The word is corrected as “absorptivity”
"absorptive" with "absorptivity"

41. page 87, line 14: HPCL should read The incorrect one, corrected as HPLC.
HPLC.

4
42. page 87, last but one line: cefditorine Name of the drug is corrected as cefditorine
mis-spelt

43. page 88, 89 , 90, 91: cefditorine mis- Name of the drug is corrected as cefditorine
spelt in many places on these pages.

44. powerful mis-spelt throughout the The word is corrected in all the places of thesis.
thesis: it must be corrected

45. page 104, 2nd para: "this work The sentence is reframed and incorporated in
provides … within the body" - very the thesis.
poor sentence
framing; reframe to read better

46. page 105, line 11 from bottom and The word is corrected as “flanked” in the thesis.
page 106, line 7: replace "planked"
with "flanked"

47. page 112, line 1: recommendations The word is corrected as “recommendations”

mis-spelt

48. the following references have been The repeated references cited in the thesis are
cited multiple times: removed and the numbers are updated in the
ref 10 - repeated as ref 70, 81; ref 83- thesis.
repeated as ref 88; ref 111- repeated
as ref 117,122.

49. all the figures are of poor quality, in All the polarograms, voltammograms and IR
several instances, they are hardly Spectra are redrawn and incorporated in the
readable; this must be taken care of. thesis.

M.Vijaya Narasimha

Prof.G.V.Subbareddy
Supervisor