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This article was downloaded by: [Gamal Saleh]On: 09 April 2013, At: 01:33Publisher: Taylor & FrancisInforma Ltd Registered in England and Wales Registered Number: 1072954 Registeredoffice: Mortimer House, 37-41 Mortimer Street, London W1T 3JH, UK
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REVIEW ON RECENT SEPARATIONMETHODS FOR DETERMINATION OF SOMEFLUOROQUINOLONESGamal A. Saleh a , Hassan F. Askal a , Ibrahim H. Refaat a & Fatma A.M. Abdel-aal aa Department of Pharmaceutical Analytical Chemistry, Faculty ofPharmacy, Assiut University, Assiut, EgyptAccepted author version posted online: 08 Aug 2012.Version ofrecord first published: 04 Apr 2013.
To cite this article: Gamal A. Saleh , Hassan F. Askal , Ibrahim H. Refaat & Fatma A. M.Abdel-aal (2013): REVIEW ON RECENT SEPARATION METHODS FOR DETERMINATION OF SOMEFLUOROQUINOLONES, Journal of Liquid Chromatography & Related Technologies, 36:10, 1401-1420
To link to this article: http://dx.doi.org/10.1080/10826076.2012.691440
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REVIEW ON RECENT SEPARATION METHODS FORDETERMINATION OF SOME FLUOROQUINOLONES
Gamal A. Saleh, Hassan F. Askal, Ibrahim H. Refaat, andFatma A. M. Abdel-aal
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy,Assiut University, Assiut, Egypt
& Fluoroquinolones (FQs) are among the most important antibacterial agents (syntheticantibiotics) used in human and veterinary medicine. They are employed against all bacterialinfections, particularly against urinary tract infections and acute respiratory diseases. In the lastdecade, there was no review covering all different analytical methods used for the determination offluoroquinolone antibiotics. The present review presented recently published different electrophoreticand chromatographic methods for determination of seven fluoroquinolones (ciprofloxacin, gatiflox-acin, levofloxacin, lomefloxacin, norfloxacin, ofloxacin, and sparfloxacin). Presented applicationsconcern analysis of chosen fluoroquinolones in pure forms, different pharmaceutical formulations,biological fluids, and environmental samples.
Keywords biological fluids, HPLC methods, electrophoretic methods, fluoroquino-lones, pharmaceutical preparations, TLC methods
INTRODUCTION
Following the discovery of nalidixic acid in 1962 by Lesher et al.[1]
numerous structural modifications have been made in the quinolinenucleus to increase antimicrobial activity and improve pharmacokineticperformance. All of these newer agents have similar mechanisms of action,but numerous derivatives of the basic 4-quinolone structure have beensynthesized in an effort to enhance the antimicrobial spectrum and phar-macological properties of these antimicrobials. Many reviews were per-formed for these drugs[2–16] but in the last few years, there has been noreview published covering all the different separation methods used forthe determination of the chosen fluoroquinolones (FQs). The high impor-tance of this class of drugs prompted us to review the most important
Address correspondence to Fatma A. M. Abdel-aal, Department of Pharmaceutical AnalyticalChemistry, Faculty of Pharmacy, Assiut University, 71526 Assiut, Egypt. E-mail: [email protected]
Journal of Liquid Chromatography & Related Technologies, 36:1401–1420, 2013Copyright # Taylor & Francis Group, LLCISSN: 1082-6076 print/1520-572X onlineDOI: 10.1080/10826076.2012.691440
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recent methods for their analysis in pure forms, in different pharmaceuti-cal dosage forms and in biological fluids. Because of the large number ofreferences that appeared as individual methods or as a part of clinicaland pharmacological studies, it is preferable to make reference only tothe most important papers.
The presented review provided a summary of important reportedmethods for seven fluoroquinolones (FQs), namely: ciprofloxacin (Cip.),gatifloxacin (Gat.), levofloxacin (Lev.), lomefloxacin (Lom.), norfloxacin(Nor.), ofloxacin (Ofl.), and sparfloxacin (Spr.).
SEPARATION METHODS
Chromatographic Methods
Thin-Layer Chromatographic Methods (TLC)TLC is one of the most widespread analytical methods used in the sep-
aration and identification of drugs. It is an inexpensive method that con-sumes only small amounts of samples and solvents. There are almost norestrictions on the solvents used and a variety of stationary phases is commer-cially available.[17] Several papers were published regarding different meth-ods for determination of FQs. Table 1 summarizes these methods.[18–31]
High Performance Liquid Chromatographic Methods (HPLC)HPLC is the most frequently applied technique for the determination
of the 4-quinolones, whether in formulations, biological fluids, animaltissues, fish feed, environmental samples, and so forth. Table 2 summarizessome of the reported methods for the analysis of 4-quinolone antibacterialin their pharmaceutical formulations, biological fluids, environmentalsamples, and so forth.[32–113]
Electrophoretic Methods
In Bulk and Pharmaceutical Dosage FormCapillary Zone Electrophoresis (CZE). Capillary electrophoresis (CE) is a
technique designed to separate species based on their size to charge ratioin the interior of a small capillary filled with an electrolyte. In 2002, Lozanoand his co-workers[114] developed a CZE method comparing the values ofdissociation constants of quinolones from mobility and spectroscopic dataobtained by capillary electrophoresis and a diode array detector. Barbosaand his co-workers[115] studied the electrophoretic behavior of quinolonesin capillary electrophoresis with the effect of pH and evaluating the ioniza-tion constants. They also studied the influence of pH and pKa values on
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TABLE
1T
LC
Met
ho
ds
for
the
Det
erm
inat
ion
of
4-Q
uin
olo
nes
inD
iffe
ren
tM
atri
ces
FQ
sM
ob
ile
Ph
ase
Ap
pli
cati
on
Det
ecti
on
Ref
.
No
r.,
Ofl
.� M
eth
ano
l:ch
loro
form
:co
nc.
amm
on
ia(5
1:34
:15,
v=v=v)
for
No
r.� E
than
ol:
con
c.am
mo
nia
(4:1
,v=v)
for
Ofl
.R
esid
ues
on
stai
nle
ssst
eel
surf
aces
Flu
or.k e
x31
3n
man
dk e
m40
0n
m
[18
,19
]
Spr.
Eth
ano
l:et
hyl
acet
ate:
1,2-
dic
hlo
roet
han
e:10
%aq
ueo
us
amm
on
ia(4
0:30
:20:
10,v=v)
Seru
man
du
rin
eF
luo
r.k e
x28
5n
man
dk e
m40
0n
m
[20
]
Spr.
Dic
hlo
rom
eth
ane:
iso
pro
pyl
alco
ho
l:25
%N
H3
(4:5
:2,v=v)
Tab
lets
vid
eod
ensi
tom
etry
atk¼
254
nm
[21
]
Ofl
.D
ich
loro
met
han
e:m
eth
ano
l:25
%N
H3
(7:5
:1.5
,v=v=v)
Tab
lets
vid
eod
ensi
tom
etry
atk¼
254
nm
[22
]
Lev
.h
emih
ydra
tesi
mu
ltan
eou
sly
wit
ho
rnid
azo
le
N-b
uta
no
l:m
eth
ano
l:am
mo
nia
(5:1
:1.5
,v=v=v)
Tab
lets
UV
298
nm
[23
]
Lev
.W
ater
:met
han
ol:
n-b
uta
no
l:am
mo
nia
solu
tio
n(5
:5:5
:0.4
,v=v)
Ph
arm
aceu
tica
lfo
rmu
lati
on
sU
V29
8n
m[2
4]
Lev
.h
emih
ydra
tesi
mu
ltan
eou
sly
wit
ham
bro
xol
hyd
roch
lori
de
Ch
loro
form
:met
han
ol:
tolu
ene:
amm
on
ia(1
0:6:
3:0.
8,v=v=v=v)
Bu
lkfo
rms
and
tab
lets
UV
254
nm
[25
]
No
r.,
Ofl
.A
qu
eou
sm
icel
leso
luti
on
of
sod
ium
do
dec
ylsu
lfat
e(S
DS)
:E
DT
A¼
0.01
:0.1
(mo
l=L
:mo
l=L
)Se
rum
and
uri
ne
Flu
or.k e
x27
8an
d28
0n
man
dk e
m
400
nm
[26
,27
]
Gat
.si
mu
ltan
eou
sly
wit
ho
rnid
azo
leN
-bu
tan
ol:
met
han
ol:
amm
on
ia(6
M)
(8:1
:1.5
,v=v=v)
Tab
lets
UV
302
nm
[28
]
Cip
.,L
om
.H
Cl
Ch
loro
form
:met
han
ol:
25%
amm
on
ia(4
3:43
:14,
v=v=v)
for
Cip
.an
d(1
0:7:
3,v=
v=v)
for
Lo
m.
HC
lP
har
mac
euti
cal
form
ula
tio
ns
UV
330
for
Cip
.28
8n
mfo
rL
om
.H
Cl.
[29
,30
]
No
r.si
mu
ltan
eou
sly
wit
hm
etro
nid
azo
leC
hlo
rofo
rm:m
eth
ano
l:d
ieth
ylam
ine:
H2O
(9:2
:0.4
:0.2
)T
able
tsU
V25
4n
m[3
1]
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TABLE
2H
PL
CM
eth
od
sfo
rth
eD
eter
min
atio
no
fF
luo
roq
uin
olo
nes
inP
har
mac
euti
cal
Fo
rmu
lati
on
san
dO
ther
Dif
fere
nt
Mat
rice
s
Dru
gsM
atri
xM
ob
ile
Ph
ase
Det
ecti
on
Ref
.
Cip
.T
able
tsan
dh
um
anp
lasm
aA
ceto
nit
rile
:2%
acet
icac
idaq
ueo
us
solu
tio
n(1
6:84
,v=v)
UV
280
nm
[32
]
Cip
.T
able
tsM
eth
ano
l:b
uff
er(0
.025
MO
rth
op
ho
sph
ori
cac
idw
ith
the
pH
adju
sted
to3.
0�
0.1
wit
htr
ieth
ylam
ine)
(40:
60,v=v)
UV
278
nm
[33
]
Cip
.,L
ev.
Ph
arm
aceu
tica
lfo
rmu
lati
on
sM
eth
ano
lan
d25
mM
ph
osp
hat
eb
uff
er(2
8:72
,v=v)
atp
H3
UV
278
nm
[34
]
Cip
.,N
or.
,O
fl.
Ph
arm
aceu
tica
lfo
rmu
lati
on
san
dh
um
anse
rum
Aw
ater
:ace
ton
itri
le(5
0:50
,v=v)
of
pH
2.9
adju
sted
wit
hp
ho
sph
ori
cac
idU
V26
0,26
5,27
0,27
5,an
d28
0n
m
[35
]
Cip
.,N
or.
,O
fl.
Sew
age
Mix
ture
of
met
han
ol,
acet
on
itri
le,
and
form
icac
idF
luo
r.27
8an
d44
5n
m,
(ESI
-MS)
[36
]
Cip
.C
atfi
shm
usc
leL
CB
uff
er(0
.1M
mal
on
ate,
50m
Mm
agn
esiu
mch
lori
de,
pH
6.5
wit
hN
H4O
H),
and
met
han
ol
Flu
or.
275
and
425
nm
[37
]
Cip
.,N
or.
Surf
ace
wat
ers
0.02
5M
ph
osp
ho
ric
acid
solu
tio
nat
pH
3.0
wit
hte
trab
uty
lam
mo
niu
mb
rom
ide
(TB
AB
)an
dm
eth
ano
l(96
0:40
,v=v)
Flu
or.
278
and
450
nm
[38
]
Cip
.,L
ev.,
Lo
m.,
No
r.P
ork
sam
ple
Ace
ton
itri
le(A
CN
)(co
nta
inin
g0.
1%o
fp
ho
sph
atic
acid
)U
V,
281
nm
[39
]
Cip
.,N
or.
Ch
icke
nm
usc
leG
rad
ien
tel
uti
on
fro
m(A
)w
ater=fo
rmic
acid
(99.
8=0.
2)an
d(B
)A
CN
(ESI
-TO
FM
S)[4
0]
Cip
.T
able
eggs
Co
mb
inin
gso
lven
tA
(25
mM
ort
ho
ph
osp
ho
ric
acid
adju
sted
top
H3.
0w
ith
NaO
H)
and
solv
ent
B(a
ceto
nit
rile
)F
luo
r.28
0an
d44
0n
m[4
1]
Cip
.C
hic
ken
mu
scle
Solv
ent
A(0
.1M
mal
on
ate,
50m
MM
gþ2,
adju
sted
top
H6.
5w
ith
con
cen
trat
edN
H4O
H)
and
solv
ent
B(m
eth
ano
l)F
luo
r.27
5an
d42
5n
m[4
2]
Cip
.,N
or.
,O
fl.
Ch
icke
nm
usc
lean
deg
gyo
lkM
ixtu
reo
f0.
1%tr
iflu
oro
acet
icac
id(T
FA)–
(AC
N)–
CH
3O
HD
AD
,27
5an
d25
5n
m[4
3]
Cip
.H
um
anh
um
or
Ace
ton
itri
le85
%:a
qu
eou
sp
ho
sph
ori
cac
id(1
5:85
,v=v)
UV
at27
8n
m[4
4]
Cip
.,G
at.,
Lev
.,L
om
.,N
or.
,Sp
r.A
qu
atic
envi
ron
men
t0.
1%A
qu
eou
sT
FAan
dac
eto
nit
rile
ESI
-MS
[45
]
Cip
.G
ilth
ead
seab
ream
Mix
ture
of
0.2%
(v=v)
form
icac
id,
met
han
ol,
and
acet
on
itri
leM
S=M
S[4
6]
Cip
.,L
ev.,
Lo
m.,
No
r.C
hic
ken
Aac
eto
nit
rile
and
wat
er(c
on
tain
ing
0.05
%fo
rmic
acid
)E
SI-M
S[4
7]
Cip
.M
ilk
CH
3O
Hþ
CH
3C
Nþ
0.2%
HC
OO
H(1
5:15
:70,
v=v)
.F
luo
r.at
275
and
[48
]
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445
nm
Cip
.W
ho
leb
loo
dC
H3O
Hþ
CH
3C
Nþ
0.2%
HC
OO
H(1
5:15
:70,
v=v=v)
.F
lou
r.at
275
and
445
nm
[49
]
Cip
.R
oas
tee
lM
eth
ano
l,ac
eto
nit
rile
and
dil
.fo
rmic
acid
(2:9
98)
(15:
15:7
0,v=v=v)
.F
lou
r.at
275
and
445
nm
[50
]
Cip
.,N
or.
,O
fl.
Mil
kM
eth
ano
l(0
.1%
form
icac
id)
and
wat
er(0
.1%
form
icac
id);
ESI
-MS
[51
]
Cip
.,N
or.
,O
fl.
Bo
vin
eli
ver
and
po
rcin
eki
dn
eyM
ixtu
reo
fT
FA0.
1%þ
CH
3C
Nþ
CH
3O
HD
AD
at27
5an
d25
5n
m[5
2]
Cip
.,N
or.
,O
fl.,
Spr.
Ch
icke
nm
usc
leC
H3O
Hþ
CH
3C
Nþ
0.2%
HC
OO
H(1
5:15
:70,
v=v=v)
ESI
-MS
[53
]
Cip
.,N
or.
Ch
icke
neg
gsM
ixtu
reo
fac
eto
nit
rile
and
0.4%
ph
osp
ho
ric
acid
–0.4%
trie
thyl
amin
e(1
5:85
,v=v)
(pH¼
2)F
luo
r.27
8an
d44
5n
m[5
4]
Cip
.,L
om
.,N
or.
Mar
ine
Pro
du
cts
0.1%
Fo
rmic
acid
,p
H2.
5,an
dac
eto
nit
rile
Flu
or.
280
and
450
nm
[55
]
Cip
.,L
ev.,
No
r.Se
rum
Wat
erso
luti
on
(1.3
1g=
Lis
ole
uci
ne
and
0.80
g=L
Cu
SO4)
and
met
han
ol
(80:
20,v=v)
Flu
or.
280
and
504
nm
[56
]
Cip
.,G
at.,
No
r.,O
fl.
Uri
ne
Ace
ton
itri
le–0
.02
mm
olL
�1
TB
AB
solu
tio
n(8
:92,
v=v,
pH
2.9)
DA
D27
7an
d29
3n
m[5
7]
Cip
.,O
fl.,
Spr.
Ro
ast
eels
CH
3O
H=C
H3C
N=0.
2%H
CO
OH
(15=
15=70
,v=v=v)
ESI
-MS
[58
]
Cip
.,L
om
.W
ater
sam
ple
s5
mm
olL
�1
BM
Im-B
F4,
and
10m
mo
lL�
1am
mo
niu
mac
etat
eat
pH
3.0
wit
h13
%(v=v)
acet
on
itri
leF
luo
r.27
8an
d44
0n
m[5
9]
Cip
.P
ork
Ace
ton
itri
le-p
ho
sph
oro
us
acid=tr
i-eth
ylam
ine
Flu
or.
280
and
450
nm
[60
]
Cip
.,L
ev.,
Lo
m.,
No
r.C
hic
ken
Ace
ton
itri
lean
dw
ater
(co
nta
inin
g0.
05%
form
icac
id)
ESI
-MS
[61
]
Cip
.G
ilth
ead
seab
ream
Mix
ture
of
0.2%
(v=v)
form
icac
id,
met
han
ol
and
acet
on
itri
leM
S=M
S[6
2]
Cip
.F
ish=sh
ellf
ish
tiss
ues
CH
3C
N-0
.05%
CF
3C
OO
H(2
5:75
,v=v)
MS=
MS
[63
]
Cip
.,N
or.
Fee
ds
Ace
ton
itri
lean
do-
ph
osp
ho
ric
acid
25m
Mat
pH¼
3F
luo
r.27
8,46
6n
mD
AD
,27
8n
m.
[64
]
Cip
.,L
ev.,
Lo
m.,
Ofl
.U
rin
ea)
0.15
MSo
diu
md
od
ecyl
sulf
ate
(SD
S),
12.5%
pro
pan
ol
and
0.5%
trie
thyl
amin
eat
pH
3.0
b)
0.05
MSD
S,12
.5%
pro
pan
ol,
and
0.5%
trie
thyl
amin
eat
pH
3.0
a)F
luo
r.28
5an
d46
5n
mb
)F
lou
r.29
5an
d48
5n
m
[65
]
Cip
.P
igti
ssu
esM
ixtu
reo
fp
ho
sph
ate
bu
ffer
(pH
3.0)
and
acet
on
itri
le(8
2:18
,v=v)
Flu
or.
278
and
450
nm
[66
]
Cip
.,L
ev.,
No
r.W
ater
sam
ple
sM
eth
ano
l=w
ater
(ad
just
edat
pH¼
2.5
wit
hac
etic
acid
;(1
5:85
,v=v)
Flu
or.
280
and
450
nm
[67
]
Cip
.,L
ev.,
Lo
m.,
Spr.
En
viro
nm
enta
lw
ater
sam
ple
sM
ixtu
reo
faq
ueo
us
solu
tio
no
f0.
25%
form
icac
idan
d10
mm
ol=
Lam
m.
acet
ate
and
acet
on
itri
leE
SI-M
S=M
S[6
8]
Cip
.,N
or.
Po
ult
rym
usc
le0.
025
mo
lL�
1H
3P
O4
solu
tio
n,
adju
sted
top
H3.
0w
ith
Flu
or.
278
and
445
nm
[69
]
(Continued
)
1405
Dow
nloa
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by [
Gam
al S
aleh
] at
01:
33 0
9 A
pril
2013
TABLE2
Co
nti
nu
ed
Dru
gsM
atri
xM
ob
ile
Ph
ase
Det
ecti
on
Ref
.
tetr
abu
tyla
mm
on
ium
hyd
roxi
de-
met
han
ol
(78:
22)
Cip
.,L
ev.
Seru
m1%
Tri
eth
ylam
ine
(pH
3.0)
:ace
ton
itri
le(8
6:14
,v=v)
Flu
or.
300
and
450
nm
[70
]
Cip
.M
ilk
25m
MP
ho
sph
ate
bu
ffer
(pH
2.5)=ac
eto
nit
rile=m
eth
ano
l(7
7:10
:13,
v=v=v)
Flu
or.
280
and
450
nm
[71
]
Cip
.,N
or.
En
viro
nm
enta
lsu
rfac
ew
ater
Ace
ton
itri
lean
d20
mM
KH
2P
O4
pH
3in
the
rati
oo
f17
%an
d83
%
(v=v)
,re
spec
tive
ly[p
Had
just
edw
ith
H3P
O4
(85%
)]D
AD
,27
0n
m[7
2]
Cip
.,N
or.
An
imal
sam
ple
sM
ixtu
reo
fac
eto
nit
rile
and
0.05
%H
3P
O4
(pH¼
2.4)
Flu
or.
278
and
445
nm
[73
]
Cip
.,L
om
.,N
or.
,O
fl.
Sed
imen
tso
fth
eP
earl
Riv
ers
Ace
ton
itri
lean
d5
mM
oxa
lic
acid
ESI
-MS
[74
]
Cip
.H
Cl
Ho
ney
25m
MP
BS
(pH
2.1)
(elu
ent
A),
met
han
ol
(elu
ent
B)
and
acet
on
itri
le(e
luen
tC
)E
SI-M
S[7
5]
Cip
.,L
om
.,N
or.
,O
fl.
Sed
imen
tso
fth
eP
earl
Riv
ers
Ace
ton
itri
lean
d5
mM
oxa
lic
acid
ESI
-MS
[76
]
Cip
.,G
at.,
No
r.B
ovi
ne
uri
ne
and
En
viro
nm
enta
lw
ater
0.1%
Fo
rmic
acid
(pH
2.6)
and
acet
on
itri
leD
AD
274–
315
nm
,F
lou
r.27
8–33
0,an
d36
8–51
5n
m
[77
]
Cip
.,O
fl.
Hu
man
seru
mA
ceto
nit
rile
–0.0
2m
olL
�1
tetr
abu
tyl
amm
on
ium
bro
mid
e(T
BA
B)
aqu
eou
sso
luti
on
(9:9
1,v=v;
pH
:2.
50)
DA
D27
7an
d29
3n
m,
resp
ecti
vely
[78
]
Cip
.,N
or.
,O
fl.
Sed
imen
tso
fth
eH
aiR
iver
,L
iao
Riv
eran
dYe
llo
wR
iver
.
Ace
ton
itri
lean
d5
mM
oxa
lic
acid
ESI
-MS
[79
]
Gat
.P
har
mac
euti
cal
form
ula
tio
ns
Ace
ton
itri
lean
d0.
05M
ph
osp
hat
eb
uff
erin
the
rati
oo
f(2
5:75
,v=v)
UV
293
nm
[80
]
Gat
.H
um
anse
rum
and
uri
ne
10m
MSD
S,10
mM
TB
AA
,an
d25
mM
citr
icac
idw
ith
50%
acet
on
itri
lein
dei
on
ized
wat
erU
V29
3n
m[8
1]
Gat
.A
qu
eou
sh
um
or
0.1
mo
l=L
Fo
rmic
acid
aqu
eou
sso
luti
on
and
acet
on
itri
lein
ara
tio
of
80:2
0(v=v)
MS
[82
]
Gat
.O
cula
rsa
mp
les
20%
Ace
ton
itri
le,
in0.
1%tr
iflu
oro
acet
icac
id(p
H3.
0)w
ith
30m
Mte
trab
uty
lam
mo
niu
mch
lori
de
UV
295
nm
,F
lou
r.34
5,an
d47
0n
m
[83
]
Gat
.,Sp
r.P
har
mac
euti
cal
form
ula
tio
ns
Met
han
ol:
0.02
5M
KH
2P
O4
adju
sted
top
H3
usi
ng
ort
ho
-ph
osp
ho
ric
acid
UV
290
nm
[84
]
Lev
.P
har
mac
euti
cal
Am
ixtu
reo
f0.
5%(v=v)
trie
thyl
amin
ein
sod
ium
dih
ydro
gen
UV
294
nm
[85
]
1406
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al S
aleh
] at
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pril
2013
form
ula
tio
ns
ort
ho
ph
osp
hat
ed
ehyd
rate
(25
mM
;p
H6.
0)an
dm
eth
ano
lL
ev.
Uri
ne
25m
MP
ota
ssiu
md
ihyd
roge
np
ho
sph
ate
(pH
adju
sted
to3.
1w
ith
ph
osp
ho
ric
acid
):ac
eto
nit
rile
(70:
30,v=v)
UV
293
nm
.[8
6]
Lev
.,L
om
.,Sp
r.E
nvi
ron
men
tal
wat
ersa
mp
les
Mix
ture
of
aqu
eou
sso
luti
on
incl
ud
ing
0.25
%fo
rmic
acid
and
10m
mo
lL�
1am
mo
niu
mac
etat
e,an
dac
eto
nit
rile
.E
SI-M
S[8
7]
Lev
.R
atp
lasm
aan
dsa
liva
Mix
ture
of
Ace
ton
itri
le:
wat
er(8
0:20
,v=v)
adju
sted
top
H3.
5b
yo
rth
op
ho
sph
ori
cac
idU
V29
6n
m[8
8]
Lo
m.,
Ofl
.P
orc
ine
tiss
ue
Solv
ent
A(0
.003
mo
l=l
H3P
O4)
and
solv
ent
B(a
ceto
nit
rile
)D
AD
280
nm
[89
]
Lo
m.,
No
r.,
Ofl
.P
har
mac
euti
cal
was
tew
ater
Mix
ture
of
met
han
ol:
wat
er:T
FA(7
0:30
:0.0
5,v=
v=v)
UV
280
nm
[90
]
No
r.C
apsu
les
Ace
ton
itri
lean
d0.
1%fo
rmic
acid
ESI
-MS
[91
]
No
r.R
awm
ater
ials
and
ph
arm
aceu
tica
lfo
rmu
lati
on
s
0.05
MN
aH2P
O4
(pH
2.5)
–ac
eto
nit
rile
(87:
13,v=v)
for
16m
in(5
8:42
,v=v)
for
9m
inD
AD
275
nm
[92
]
No
r.H
um
anp
lasm
aA
ceto
nit
rile
:met
han
ol:
aqu
eou
sco
mp
on
ent
(70:
15:1
5,v=v=v)
Flu
or.
268
and
445
nm
[93
]
No
r.H
um
anp
lasm
aM
ixtu
reo
fp
ho
sph
ate
bu
ffer
:ace
ton
itri
le(8
5:15
,v=v)
Flu
or.
300
and
450
nm
[94
]
No
r.R
iver
cru
cian
carp
0.05
mo
l=L
Fo
rmic
acid
:tr
ieth
ylam
ine
bu
ffer
:ace
ton
itri
le(8
0:20
,v=v)
Flu
or.
280
and
450
nm
[95
]
No
r.H
um
anp
lasm
a14
%A
ceto
nit
rile
inb
uff
erso
luti
on
;aq
ueo
us
ph
ase
was
pre
par
edb
ym
ixin
g2
go
fci
tric
acid
,2
gso
diu
mac
etat
e,an
d1
mL
of
trie
thyl
amin
ein
1L
of
Mil
li-Q
wat
er
Flu
or.
330
and
440
nm
[96
]
No
r.gl
uta
mat
eP
har
mac
euti
cal
form
ula
tio
ns
0.02
5m
ol=
Lp
ho
sph
ori
cac
id(p
H3.
0,ad
just
edw
ith
trie
thyl
amin
e):a
ceto
nit
rile
(84:
16,v=v)
UV
278
nm
[97
]
Ofl
.T
able
tsM
eth
ano
lan
d25
mM
ph
osp
hat
eb
uff
er40
:60%
(v=v)
pH
adju
sted
to5.
5u
sin
go
rth
op
ho
sph
ori
cac
idD
AD
290
nm
[98
]
Ofl
.H
on
eyC
H3C
N(2
5%)
and
0.05
%(T
FA)
(75%
)E
SI-M
S[9
9]
Ofl
.M
ilk
10m
Mac
etic
acid
:so
diu
mac
etat
eb
uff
er(p
H5.
4)=ac
eto
nit
rile
(75:
25,v=v)
Ele
ctro
gen
erat
edC
hem
ilu
min
esce
nce
det
ecto
r(E
CL
)
[10
0]
Flu
oro
qu
ino
lon
esP
har
mac
euti
cal
form
ula
tio
ns
Ace
ton
itri
le:m
eth
ano
l:1%
TFA
(4:7
:89,
v=v=v)
Flu
or.
280
and
450
nm
[10
1]
Flu
oro
qu
ino
lon
esH
um
anu
rin
eM
ixtu
reo
fac
eto
nit
rile
:0.
02m
ol=
LT
BA
B(9
:91,
v=v
adju
stin
gp
H2.
87b
yT
FAb
uff
er)
DA
D28
2n
m[1
02
]
Flu
oro
qu
ino
lon
esF
ish
mu
scle
Mix
ture
of
met
han
ol-m
agn
esiu
mch
lori
de
and
mal
on
icac
idb
uff
erU
V28
2n
m[1
03
]
Flu
oro
qu
ino
lon
esB
ovi
ne
mil
kM
ob
ile
ph
ase
com
po
nen
tA
was
am
eth
ano
l:ac
eto
nit
rile
(70:
30,v=v)
ESI
-MS
[10
4]
(Continued
)
1407
Dow
nloa
ded
by [
Gam
al S
aleh
] at
01:
33 0
9 A
pril
2013
TABLE2
Co
nti
nu
ed
Dru
gsM
atri
xM
ob
ile
Ph
ase
Det
ecti
on
Ref
.
mix
ture
,w
hil
eco
mp
on
ent
Bw
asw
ater
Flu
oro
qu
ino
lon
esE
ggs
A:
(aq
ueo
us
form
icac
idso
luti
on
,0.
1%),
B:
(org
anic
form
icac
idso
luti
on
,0.
1%),
and
C:
(met
han
ol)
ESI
-MS
[10
5]
Flu
oro
qu
ino
lon
esIn
fan
tfo
od
sA
CN=o
:ph
osp
ho
ric
acid
50m
Mp
H3.
0(8
0:20
,v=v)
MS=
MS
[10
6]
Flu
oro
qu
ino
lon
esSe
dim
ents
of
Hai
he
Riv
erA
ceto
nit
rile
-0.3%
form
icac
idM
S=M
S[1
07
]
Flu
oro
qu
ino
lon
esB
aby
foo
ds
A:
(H2O
wit
h0.
1%T
FA),
B:
(ace
ton
itri
lew
ith
0.1%
TFA
),an
dC
:(m
eth
ano
l)F
luo
r.28
0,44
0,an
d51
5n
m
[10
8]
Flu
oro
qu
ino
lon
esE
ggs
An
aqu
eou
sso
luti
on
of
0.01
mo
lL�
1o
xali
cac
idþ
acet
on
itri
leF
lou
r.26
3–29
7an
d36
–507
nm
[10
9]
Flu
oro
qu
ino
lon
esM
ilk
10m
Mac
etic
acid
:so
diu
mac
etat
eb
uff
er(p
H5.
4)=ac
eto
nit
rile
(75:
25,v=v)
Ele
ctro
gen
erat
edC
hem
ilu
min
esce
nce
det
ecto
r(E
CL
)
[11
0]
Flu
oro
qu
ino
lon
esR
awb
ovi
ne
and
skim
med
mil
kG
rad
ien
tel
uti
on
wit
h(A
)u
ltra
-pu
rew
ater
and
(B)
acet
on
itri
leb
oth
acid
ifie
dw
ith
0.2%
form
icac
idM
S=M
S(t
and
emm
ass
spec
tro
met
ry)
[11
1]
Flu
oro
qu
ino
lon
esM
usc
le,
live
r,ki
dn
eyo
fsw
ine,
bo
vin
e,ch
icke
n,
and
fish
Ath
ree
grad
ien
tsy
stem
wit
hm
eth
ano
l=ac
eto
nit
rile=0.
02M
citr
icac
idan
d0.
03M
amm
on
ium
acet
at.
UV
278
nm
,M
S=M
S(t
and
emm
ass
spec
tro
met
ry)
[11
2]
Flu
oro
qu
ino
lon
esE
nvi
ron
men
tal
wat
ersa
mp
les
Ace
ton
itri
le(A
)an
d0.
1%fo
rmic
acid
solu
tio
nco
nta
inin
g0.
01m
olL
�1
TB
AB
(B)
UV
280
nm
[11
3]
Ab
bre
viat
ion
s:A
CN
,A
ceto
nit
rile
;D
AD
,D
iod
arra
yd
etec
tor;
ESI
-TO
FM
S,E
lect
rosp
ray
Ion
izat
ion
-Tim
eo
fF
ligh
tM
ass-
Spec
tro
met
ry;
Flu
or.
,F
luo
resc
ence
;G
C-M
S,G
asC
hro
mat
ogr
aph
y-M
ass
Spec
tro
met
ry;
HP
LC
,H
igh
Per
form
ance
Liq
uid
Ch
rom
ato
grap
hy;
LC
-MS,
Liq
uid
Ch
rom
ato
grap
hy-
Mas
sSp
ectr
om
etry
;P
BS,
Ph
osp
hat
eb
uff
ered
sali
ne;
TB
AB
,T
etra
bu
tyla
mm
on
ium
bro
mid
e;T
FAT
rifl
uo
roac
etic
acid
.
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2013
electrophoretic behavior of quinolones in aqueous and hydro-organicmedia[116] and studied a model of electrophoretic behavior in order tooptimize the separation of zwitterionic substances by capillary electropho-resis. The model considers the effect of ionic strength and can be appliedto zwitterionic substances with very close pKa values. The model was testedto obtain the optimum pH values for the separation of a series of eightquinolones.[117] The same workers presented a paper in which dissociationconstants of quinolones in MeOH-water mixtures were obtained usingcapillary electrophoresis. The method is based on a model that relateselectrophoretic mobility of the solute with pH.[118]
There are several CZE methods were reported for determination of FQsin different dosage forms and are summarized in Table 3.[119–128]
Electrokinetic Capillary Chromatography (ECC). A separation techniquebased on a combination of electrophoresis and interactions of the analyteswith additives (e.g., surfactants), which form a dispersed phase moving at adifferent velocity. In order to achieve separation either the analytes or thissecondary phase should be charged.[129]
1. Micellar electrokinetic capillary chromatography (MEKC)A special case of electrokinetic chromatography, in which the secondaryphase is a micellar dispersed phase in the capillary.[129] MEKC hasenabled the separation of electrically neutral analytes. It can be perfor-med by adding an ionic micelle to the running solution of CE withoutmodifying the instrument. Its separation principle is based on the differ-ential migration of the ionic micelles and the bulk running buffer underelectrophoresis conditions and on the interaction between the analyteand the micelle. Hence, MEKC’s separation principle is similar to thatof chromatography. MEKC is a useful technique particularly for the sep-aration of small molecules, both neutral and charged, and yieldshigh-efficiency separation in a short time with minimum amounts ofsample and reagents.[130] Recently, in 2012, an MEKC method was devel-oped using [BMIM] PF6 (1-butyl-3-methylimidazolium hexafluoropho-sphate) as a modifier for separating 4 fluoroquinolone compounds(ciprofloxacin, gatifloxacin, ofloxacin, and norfloxacin). The effects ofseveral parameters on the separation selectivity, such as pH, concentra-tion of background electrolyte, concentration ratio and amount of[BMIM] PF6, and (sodium dodecyl sulfate) SDS were investigated.Under the optimal conditions of 10 mmol L�1 sodium borate, pH 7.1,1.7% (w=w) SDS, and 1.5% (w=w) [BMIM] PF6 with 18 kV as the runningvoltage, the 4 investigated quinolone compounds were baseline separa-ted within 15 min. The selectivity of the developed method differed fromthat of the simple SDS micelles system containing no ionic liquid.[131]
Fluoroquinolone Separation Method Review 1409
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pril
2013
2. Microemulsion Electrokinetic Capillary Chromatography (MEEKC)MEEKC is a special case of electrokinetic chromatography, where amicroemulsion is employed as the dispersed phase.[129] In 2008,Shou-Lian et al.[132] developed a method using sodium dodecylsulfate(SDS) as the surfactant, and an exhaustive study of the influence ofbuffer pH, phosphate concentration, SDS concentration, co-surfactantconcentration, oil concentration, and temperature was carried out.Baseline separation of seven FQs was achieved in a carrier electrolytecontaining 1% (v=v) heptane, 100 mmol=L SDS, 10% (v=v) 1-butanoland 8-mmol=L phosphate-sodium tetraborate buffer at pH 7.30, andOfl. was used as an internal standard.
TABLE 3 Capillary Electrophoresis Methods for the Determination of 4-Quinolones in DifferentDosage Forms
FQs Conditions Detection Ref.
Cip., Nor., Ofl. 50 mM carbonate buffer at pH 9.2 with anapplied voltage of 20 kV at 30�C
UV 280 nm, Fluor.kex 325 nm,and kem at 420 nm
[119]
Cip. Phosphate buffer pH 6.0 that is supplementedwith 0.075 M pentane-1-sulfonic acid sodiumsalt, applied voltage of 15 kV
UV 280 nm [120]
Cip., Lom., Nor.,Ofl., Spr.
65 mM Sodium borate=35 mM sodiumdihydrogen phosphate=60 mM sodiumcholate of pH 7.3 in acetonitrile (72:28) asrunning buffer, applied voltage of þ27 Kv
UV 275 nm [121]
Cip., Gat., Lev., Spr. 25 mmol=L Tris=hydrochloride and 15 mmol=Lsodium tetraborate buffer mixture resulting inpH 8.87 with an applied voltage of þ25 kV
UV 282 nm [13]
Ofl. 50 mM sodium phosphate buffer, pH 2.8containing 4.0% methyl b-cyclodextrin as achiral selector, applied voltage 20 kV,temperature 25�C
UV 280 nm [122]
Cip. 60 mmol=L sodium phosphate plus 20 mmol=Lsodium tetraborate, pH 8.5; voltage 24 kV andtemperature, 26�C
UV 270 nm [123]
Spr. 25 mM H3PO4-NaOH running buffer (pH 8.5),25�C; applied voltage 12 kV
UV 254 nm [124]
Ofl. Simultaneouslywith ornidazole
25 mmol=L Phosphoric acid adjusted with 1 MTris buffer to pH 8.5, with 20 kV appliedvoltage
UV 230 nm [125]
Lom. 6.0 mmol=L Lactic acid and 5.0% C2H5OH atapplied voltage of 26.0 kV
High frequencyconductivitydetection
[126]
Cip., Nor., Ofl. Sodium phosphate buffer, pH 7.0, 125 mM, with22 kV applied voltage
UV 214 nm [127]
Nor. and its inactivedecarboxylateddegradant
10 mmol l�1 phosphate buffer at pH 2.5 withapplied voltage of 25 kV and at 25�C
DAD 301 and 285 nmfor the intact drugand the degradant,respectively
[128]
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In Biological FluidsCapillary Zone Electrophuresis (CZE). In 2000, Georg Hempel[133] pub-
lished a review discussing strategies to improve the sensitivity in capillary
TABLE 4 Capillary Electrophoresis Methods for the Determination of 4-Quinolones in DifferentBiological Fluids and Environmental Samples
FQs Matrix Conditions Detection Ref.
Cip., Lom.,Nor., Ofl.
Chicken, henand swinetissues
Buffer solution of 25 mM TRIS,40 mM boric acid, 2 mM sodiumphosphate, and 2.5 mM sodiumtetraborate decahydrate (pH 7.48)with applied voltage of 15 kV at22� 0.1�C
UV 280 nm [134]
Gat., Lom.,Nor., Ofl.Spr.
Human serum 12 mM Disodiumtetraborate-phosphate buffer (pH9.08) containing 5.2mg=L silicananoparticles as additive withþ10 kV applied voltage
UV 254 nm [135]
Lev. Human urine 60 mM hydroxylpropyl-b-cyclodextrin(HP-b-CD) in 50 mM phosphatebuffer at pH 2.30, with appliedvoltage of 15 kV
Fluor. kex 292 nmand kem at495 nm
[136]
Lom., Nor.,Ofl.
Pig plasma Buffer solution of 40 mM sodiumtetraborate at pH 8.1 containing10% (v=v) methanol, with appliedvoltage of 30 kV at 30�C
DAD 260 nm [137]
Cip. Chicken muscle Diethylmalonic buffer at pH 8.2,applied voltage of 20 kV
�UV 275 nm�LIF using HeCd
laser(kex¼ 325 nm)
[138,139]
Cip., Gat. Chicken tissue Buffer solution of 10 mM tartaric acid,14 mM sodium acetate and 15%(v=v) methanol at pH 3.8 withapplied voltage of 13 kV
Contactlessconductivitydetection
[140]
Cip., Lom.,Nor., Ofl.
Bovine rawmilk, pigkidney, andwater samples
125 mM Phosphoric acid solutionadjusted to pH 2.8 with 4 M sodiumhydroxide with 36% methanol withapplied voltage of 26 kV
LIF using aHeCd laser(kex¼ 325 nm)
[141,142]
Cip. Human urine Buffer solution of sodium tetraborate(50 mM) at pH 9.0 with appliedvoltage of 30 kV
UV 260 nm [143]
Lom., Nor.,Ofl.
Blood andsurface watersamples
50 mM H3PO4 adjusted to pH 7.55–acetonitrile (60:40, v=v) withapplied voltage of 20 kV
Fluor. kex 278 nmand kem at445 nm
[144]
Cip., Gat.,Lom., Ofl.
Porcine tissues Buffer solution of 25 mM NaH2PO4,25 mM Na2B4O7, and 25 mMH3BO3 (pH 9.0) with appliedvoltage of 20 kV
DAD 280 nm [145]
Fluoroquino-lones
Chicken liver Buffer solution of 40 mmol=LNa2HPO4 - 20 mmol=L citric acid atpH 8.47 with applied voltage of22 kV at 25�C
UV 262 nm [146]
Fluoroquinolone Separation Method Review 1411
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electrophoresis for the analysis of drugs in biological fluids especially forblood or plasma samples. The sensitivity is not sufficient to quantify drugsand their metabolites as they often need to be quantified in the lower mg=Lrange. To overcome this limitation and to increase the sensitivity, two stra-tegies were applied: first, to increase the amount of analyte added to thecapillary and, second, to increase the sensitivity on the detector site. Toimprove the sensitivity on the detector site, alternative detection techniquesto UV detection, for example, laser-induced fluorescence detection (LIF)or mass spectroscopy (MS), can be applied.[133] Many subsequent papersutilizing this strategy to improve the sensitivity of the method were publi-shed. Several CE papers were developed for determination of fluoroquino-lones and summarized in Table 4.[134–146]
Electrokinetic Capillary Chromatography (ECC)Micellar Electrokinetic Capillary Chromatography (MEKC). Table 5 summari-
zes the different methods for determination of the studied FQs using micel-lar electrokinetic capillary chromatography in different biological fluids.
Microemulsion Electrokinetic Capillary Chromatography (MEEKC). A simple,reliable microemulsion electrokinetic chromatography (MEEKC) methodwas developed for the simultaneous separation of some fluoroquinolones(FQs). The best separation was achieved in a carrier electrolyte containing1% (v=v) heptane, 100 mmol=L sodium dodecyl sulfate (SDS), 10% (v=v)1-butanol, and 8 mmol=L phosphate-sodium tetraborate buffer at pH7.30. The proposed method was directly applied to the determination ofCip. and Lom. in urine samples of subjects administered either with Cip.or Lom.[149]
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