Analysis of pharmaceuticals in waste waters Table 1

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Institut für Energie- und Umwelttechnik e. V. (IUTA)
Dr. Jochen Türk, 21.01.2009
Analysis of pharmaceuticals in waste waters
Table 1: Parameter of the final method for the manual and for the automatic SPE
apparatus
Step
Automatic
Manual
Pre-wet step 1
MeOH
2*20 mL MeOH
Soak time
1 min.
5 min.
Air dry time
4 sec.
0 sec.
water, pH 3
2*20 mL water, pH 3
Solvent soak time
1 min.
5 min.
Air dry time
4 sec.
Pre-wet step 2
Pre-wet step 2
water, pH 3
2*20 mL water, pH 3
Solvent soak time
1 min.
5 min.
Air dry time
4 sec.
Wash step
5% MeOH, pH 2
5% MeOH, pH 2
Solvent soak time
30 sec.
30 sec.
Air dry time
30 sec.
Air dry time for filtered disks
5 min.
5 min
Rinse step 1
MeOH
8mL MeOH
Solvent soak time
5 min.
5 min.
Air dry time
10 sec.
Rinse step 2
MeOH
8mL MeOH
Solvent soak time
5 min.
5 min.
Air dry time
10 sec.
Rinse step 3
E.A.
8 mL E.A.
Solvent soak time
5 min.
5 min
Air dry time
5 min.
E.A.: ethyl acetate
© IUTA e.V., 2009
Page 1 of 5
Strata X
Strata XL
HR-X
H2O phobic
Polar plus
180
160
Recovery rate [%]
140
120
100
80
60
40
20
ca
rb
am
az
ep
in
ce
e
fu
ro
x
im
ci
pr
e
of
lo
xa
cl
ar
ith cin
ro
m
cl
yc
of
in
cy
ib
r
cl
op ic a
c
ho
sp id
ha
m
id
di
e
cl
of
en
er
ac
yt
hr
er
yt
om
hr
om yci
n
yc
in
-H
20
ib
up
ro
f
ifo en
sfa
m
id
m
e
et
op
ro
lo
l
of
lo
xa
ci
pr
op n
an
ro
ol
xi
ol
th
ro
m
yc
su
lfa in
di
su
lfa azin
e
m
su
eth
lfa
az
m
eth ine
ox
az
ol
e
0
Figure 1: Recovery rates and standard deviations for different SPE-materials
Experimental conditions: c = 200 ng/mL, V = 200 mL, pH = 2, E.S, elution: 28 mL MeOH, n = 3
140
E.S
I.S
120
Recovery rate [%]
100
80
60
40
20
ca
rb
am
az
ep
in
ce
e
fu
ro
x
cl
im
ar
e
ith
ro
m
yc
cl
in
of
ib
cy
r
ic
cl
op
ac
ho
id
sp
ha
m
id
e
di
cl
of
e
n
er
ac
yt
hr
er
om
yt
hr
yc
om
in
yc
in
de
hy
.
ib
up
ro
fe
n
ifo
sfa
m
id
m
e
et
op
ro
lo
pr
l
op
an
ol
ro
ol
xi
th
ro
m
yc
su
in
lfa
di
az
su
in
lfa
e
m
eth
su
lfa
az
in
m
e
eth
ox
az
ol
e
0
Figure 2: Recovery rates using the internal standard and the external standards
Experimental conditions: c=200 ng/mL, V=200 mL, pH=3, E.S and I.S., elution 3*7.5 1st +2nd MeOH,
rd
3 EA, Pres=-17 psi, soak time 5 min, n=3; Bakerbond speedisk H2O phobic
© IUTA e.V., 2009
Page 2 of 5
200 mL
500 mL
1000 mL
160
140
Recovery rate [%]
120
100
80
60
40
20
ca
rb
am
az
e
ce pine
fu
ro
cl
xi
ar
ith me
ro
m
cl
y
o
cy
fib cin
cl
op ric a
ho
c
sp id
ha
m
id
di
e
cl
of
er
en
y
a
er
yt thro c
hr
m
om
y
yc cin
in
de
h
ib
up y.
ro
ifo fen
sfa
m
i
m
e t de
op
r
pr olo
l
op
ro ano
xi
lo
th
ro l
m
y
su
lfa cin
d
su
lfa iazi
ne
m
su
lfa etha
z
m
eth ine
ox
az
ol
e
0
Figure 3: Recovery rates for different volumes of spiked samples
Experimental conditions: c = 200 ng/mL, V = 200, 500 and 1,000 mL, pH = 3, E.S., elution 3*7.5
mL,1st +2nd MeOH, 3rd EA, Pres = -17 psi, soak time 5 min. Bakerbond speedisk H2O phobic
© IUTA e.V., 2009
Page 3 of 5
Contrast media:
SPE-Material: Biotage ISOLUTE ENV+ (200 mg/6mL)
Biotage AB
Kungsgatan 76
SE-753 18 Uppsala
Sweden
Tel. +46 1856 5710
Fax: +46 1856 5705
e-mail: [email protected]
Helmut Fritz
Biotage GmbH
Phone: +49 (0)7621 161 49 78
[email protected]
100
Iopromid
90
Iopamidol
Iomeprol
Amidotrizoic acid
Recovery rate [%]
80
70
60
50
40
30
20
10
0
1
2
3
4
Sample
FIGURE 4. RCM recovery rate for the SPE-DEX® 4790 automatic system
© IUTA e.V., 2009
Page 4 of 5
WATER SAMPLE
200ml
acidulated to pH 3 with hydrochloric acid
SOLID PHASE EXTRACTION
Prewet Step 1
Methanol / Acetonitrile (v/v; 50/50)
Soak Time 5:00 min
Air Dry Time 0:12 min
Prewet Step 2
Millipore water pH 3
Soak Time 0:30 min
Sample Loading
Rinse Step 1
Methanol
Soak Time 2:30 min
Rinse Step 2
Methanol
Soak Time 0:10 min
Solvent dry off
Nitrogen stream, 40 °C hot plate
Sample absorption
Methanol / Water (v/v; 5/95), 1 mL
HPLC-MS/MS
Sample volume 1000µL
© IUTA e.V., 2009
Page 5 of 5

Analysis of pharmaceuticals in waste waters Table 1

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