strata-X - Separations

patent pending
Selective Simple Versatile SPE
Now It’s Possible!!
SELECTIVE
p. 1
SIMPLE
p. 13
VERSATILE
p. 17
4
SELECTIVE
• Eliminates the need for
screening multiple SPE
sorbents
• Multimode retention
mechanisms allow for
selective retention and
elution
• Improved retention for
analytes that have polar or
ion functionality
1
Nortriptyline
Nortriptyline
Nortriptyline
Nortriptyline
Doxepin
Doxepin
Doxepin
Doxepin
Procainamide
Procainamide
Nordoxepin
Procainamide
Procainamide
Cimetidine
Cimetidine
Amitriptyline
Cimetidine
Cimetidine
Acetaminophen
Acetaminophen
Nortriptyline
Acetaminophen
Acetaminophen
Theobromine
Theobromine
Doxepin
Theobromine
Theobromine
Theophylline
Nordoxepin
Theophylline
Procainamide
Theophylline
Theophylline
Caffeine
Amitriptyline
Caffeine
Cimetidine
Caffeine
Caffeine
Revolutionary Polymeric Technology
Polars
strata-X -patent pending reversed phase
Reversed Phase
sorbent for extraction of polar and nonpolar compounds
BASES
Ibuprofen
Nortriptyline
CONDITIONS
Method:
Analytes spiked in porcine serum at
concentration of 0.5 or 1.0µg/mL.
The strata-X method was used.
Contact Phenomenex for more
complete method details.
2
PHENOMENEX • WEB: www.phenomenex.com
NEUTRALS
Ibuprofen
Acetaminophen
ACIDS
Ibuprofen
Ibuprofen
Naproxen
Doxepin
Naproxen
Theobromine
Naproxen
Naproxen
Fenoprofen
Procainamide
Fenoprofen
Theophylline
Fenoprofen
Fenoprofen
Indomethacin
Cimetidine
Indomethacin
Caffeine
Indomethacin
Indomethacin
Acetaminophen
Ibuprofen
Theobromine
Naproxen
Revolutionary Polymeric Technology
Bases
strata-X-C patent pending mixed-mode
Ion Exchange
cation exchange sorbent for extraction
of basic compounds
Acrylamide
Acrylamide
Neurotoxin
Neurotoxin
Verapamil
Verapamil
Antidepressant
Antidepressant
Pseudoephedrine
Pseudoephedrine
Doxepin
Doxepin
TCA TCA
Phenylpropanolamine
Phenylpropanolamine
Naproxen
Naproxen
NSAID NSAID
Acetaminophen
Acetaminophen
Diphenhydramide
Diphenhydramide
0
Analgesic
Analgesic
Codeine
Codeine
Antihistamine
Antihistamine
Chlorpheniramine
Chlorpheniramine
Metoprolol
Metoprolol
Diazepam
Diazepam
Propranolol
Propranolol
Flunitrazepam
Flunitrazepam
The mixed-mode functionality
and wide pH range of this sorbent
makes strata-X-C extremely
versatile for toxicological and
pharmaceutical analyses. Contact
Phenomenex for more complete
method details.
Decongestant
Decongestant
Beta Blockers
Beta Blockers
Phencyclidine
Phencyclidine
Benzodiazapene
Benzodiazapene
Drugs ofDrugs
Abuse
of Abuse
Flurazepam
Flurazepam
Methadone
Methadone
Bromazepam
Bromazepam
Methamphetamine
Methamphetamine
200 4020 6040 8060 100
80 100
% Recovery
% Recovery
0
200 4020 6040 8060 100
80 100
% Recovery
% Recovery
PHENOMENEX • WEB: www.phenomenex.com
3
strata-X: Improved Recovery for Substituted Aromatics
The multimode retention mechanism
of strata-X includes hydrophobic, polar
Phenols from Water
TN-001
and π-π. The polar and π-π retention
mechanisms of strata-X gives consis-
Higher analyte recoveries than traditional SPE sorbents
100
tuted aromatic analytes in comparison
90
to traditional reversed phase sorbents
80
which retain analytes primarily by
70
hydrophobic interaction.
% Recovery
tently improved recoveries for substi-
OH
OH
OH
Br
60
50
OH
OH
Br
Br
OH
OH
Br
F
O
F
Cl
Cl
Br
Br
A. Phenol
40
B. 2,4,6-Tribromophenol
30
OHOH
OH
20
Br
OHOH
OH OH
Br
Br
F Br
O
OH OH
OH
OH
Cl
F
Cl
ClCl
N+
Cl
10
0
A
B
C
D
E
SPE CONDITIONS
Sorbent: strata-X 500mg/6mL
Strata SDB-L 500mg/6mL
Order No.: 8B-S100-HCH
8B-S014-HCH
Condition: 5mL methanol
Equilibrate: 5mL water
Load: 500mL of sample (loaded in a OH
OH Br
continuous fashion)
Elute: 5mL acetone, followed by 5mL
methylene chloride
Drying: extracts were dried using anhydrous
sodium sulfate concentrated to 0.5mL
4
PHENOMENEX • WEB: www.phenomenex.com
F
G
strata-X
OH
OH
Br
H
SDB
OH
OH
Br
OH
Br
F
Br
OH
Cl
F
Cl
OH
OH
OH
OH
Cl
O
OH
N+
Cl
O-
N+
Cl
O-
O
OH
O
OH
O
O-
N+
O
N+
N+
O
O
F. 2-Nitrophenol
OH
O-
O
OH
N+
OH
O-
N+
O-
G. 2,4-Dinitrophenol
O
N
-
Cl
O-
Cl
OH
N+
N+
O-
O
OH
O
N+
OH
O
Br
Cl
E. 2,4,6-Trichlorophenol
Cl
Br
O
OH
Cl
Cl
Cl
Cl
Cl
Cl
Cl
F
Cl
D. 2-Chlorophenol
OH
OH
OH
OH
OH
Br
F
GC Column: Zebron™
ZB-5 Br Br
Br
Dimension: 30m x 0.25mm x 0.25µm
Order No.: 7HG-G002-11
Br
Injection: 1µL at 250˚C in 11:1 split
Br ratio
Carrier Gas: Helium
Oven Program: 40˚C to 325˚C, at 9˚C/min
OH
OH
Detention:OH MS in selective
ion mode OH
Cl
Br
C. 2-Fluorophenol
N+
O-
H. o-Cresol
Cl
O-
O
+
O-
O-
Diuretics from Serum
CN-009
2
93%
100
3
97%
90
1
Over 90%
recovery for
substituted
aromatics
80
A
0
2
4
6
8
10
12
14
70
% Recovery
B
60
50
40
min
30
SPE CONDITIONS
Sorbent:
Order No:
Condition:
Equilibrate:
Load:
strata-X 30mg/1mL
8B-S100-TAK
1mL methanol
1mL water
1mL porcine spiked with analyte and IS
(1.0 mg/mL Sulfaquinoxaline) diluted
1:1 with water
Wash: 1mL 5% methanol in water
Elute: 1mL methanol
Evaporate: under slow stream of N2 and
reconstitute in 200µL mobile phase
20
10
HPLC Column:
Order No:
Sample:
Mobile Phase:
SynergiTM Max-RP 4µ 150 x 4.6mm
00F-4337-E0
50µL of reconstituted extract
A: 20mM KH2PO4 (pH 2.5)
B: methanol
Gradient: A/B (95:5) to A/B (20:80) in 15 min
Flow rate: 1.0mL/min
Temperature: 25°C
Detector: UV@254nm
Peaks: 1.Hydrochlorothiazide
2. Sulfaquinoxaline (IS)
3. Furosemide
Chromatogram of Extracts:
A) Blank
B) Spiked Sample
A
0
O
O
NH2
O
NH2
S
O
S
O
O
O
S
Cl
Cl
B
O
S
NH
NH
NH
A. Hydrochlorothiazide
O
O
NH
NH
O
NH
O
NH2
S NH2
S
O
O
O
O
B. Furosemide
PHENOMENEX • WEB: www.phenomenex.com
5
strata-X: Enhanced Retention for Polar Analytes
strata-X is a surface modiﬁed styrene
divinylbenzene polymer, this gives an
Extraction of Polar Steroids from Serum
SPE sorbent that has superior H-bonding
CN-008
3
1
capabilities for enhanced retention of
94%
100
polar analytes. This can be very power2
ful for applications that require simulta-
90
4
H-bonding
provides
enhanced
polar retention
80
% Recovery
neous extraction of polar analytes (Log
99%
P<3) from non-polar parent compounds
(Log P>3).
70
60
50
40
30
20
SPE CONDITIONS
Sorbent:
Order No.:
Condition:
Equilibrate:
Load:
Wash:
Elute:
Evaporate:
6
PHENOMENEX • WEB: www.phenomenex.com
strata-X 30mg/1mL
8B-S100-TAK
1mL methanol
1mL water
1mL porcine spiked with analyte
1mL 5% methanol in water
1mL methanol
add 25µL of 0.1mg/mL butyl paraben
(external standard) dry down under
slow stream of N2 and reconstitute in
200µL acetonitrile
A
10
B
HPLC Column: SynergiTM Max-RP 4µ 150 x 4.6mm
SecurityGuard™ C18 4 x 3.0mm
Order No.: 00F-4337-E0 and AJ0-4287
Sample: 50µL of reconstituted extract
Mobile Phase: A: 20mM KH2PO4 (pH 7.0)
B: methanol
Gradient: A/B (35:65) in 20 min
Flow rate: 1.0mL/min
Temperature: 25°C
Detector: UV @ 254nm
Peaks: 1. Prednisolone
2. Betamethasone
3. Butyl Paraben (external std)
4. Betamethasone Valerate
O
Chromatogram of Extracts:
A) Blank B) Spiked Sample
A
0
B
O
OH
OH
OH
O
OH
H
H
H
H
O
A. Prednisolone
O
OH
OH
OH
O
OH
H
H
H
Log P 1.62
OH
OH
H
H
H
O
B. Betamethasone
H
Log P 1.94
O
H
OH
OH
Rapid Clean Up of Acyclovir (Log P -1.56)
100
TN-009
92%
98%
90
Superior
selectivity for
polar analytes
% Recovery
80
70
60
50
40
30
20
10
0
A
B
ON-LINE SPE CONDITIONS
Cartridge:
Order No.:
Mobile Phase:
Flow Rate:
strata-X 20 x 2.0mm cartridge plus holder
00M-S033-B0-CB
A: water; B: acetonitrile
Pump 1 3mL/min, cartridge
Pump 2 1mL/min, analytical column
Load: Pump 1 100% A (cartridge)
Sample: Pump 2 80% B: 20% A
ANALYTICAL COLUMN
HPLC Column:
Order No.:
Mobile Phase:
Flow rate:
Detection:
Sample :
Luna™ 3µ NH2 50 x 3.0mm
00B-4377-Y0
80% B: 20% A
1.0mL/min
MS in ESI-Negative mode m/z 100-400
A - Acyclovir 40ng/1mL
B - Acyclovir 20ng/1mL
Note: no buffers are used in this method
PHENOMENEX • WEB: www.phenomenex.com
7
strata-X-C: Extremely Clean Extracts
strata-X-C has a strong cation exchange
group uniformly bonded on the polymer-
Methadone from Urine
CN-014
ic surface unlike traditional silica-based
mixed mode sorbents that are blended,
completely eliminating recovery or reprochange mechanism gives consistent and
1
95%
100
100% organic
wash results in clean extracts
ducibility problems. The strong cation ex-
90
80
2
% Recovery
extremely clean extracts from biological
matrices such as plasma and urine since
hydrophobic contaminants can be com-
70
60
50
40
pletely removed by using 100% organic
30
wash solvents.
B
A
0
2
4
6
8
10
12
20
10
A
0
min
SPE CONDITIONS
Sorbent:
Order No:
Condition:
Equilibrate:
Load:
Wash 1:
Wash 2:
Elute:
Evaporate:
8
PHENOMENEX • WEB: www.phenomenex.com
strata-X-C 60mg/3mL
8B-S029-UBJ
2mL methanol
2mL water
3mL urine spiked with analytes and
IS (0.5µg/mL); dilute 1:1 with 100mM
KH2PO4 (pH 6); acidiﬁed with 2%
phosphoric acid
2mL 0.1N HCI
2mL methanol
2mL 5% NH4OH/methanol
Dry down and reconstitute with
200µL mobile phase
HPLC Column:
Order No:
Sample:
Mobile Phase:
SynergiTM Max-RP 4µ 150 x 4.6mm
00F-4337-E0
50 µL of reconstituted urine extract
A: 0.1% TFA in water pH (2.1)
B: acetonitrile
A/B (65:35)
Flow rate: 1.0mL/min
Temperature: 25°C
Detector: UV@210nm
Peaks: 1. Estazolam (IS)
2. Methadone
Chromatogram of Extracts:
A) Blank B) Spiked Sample
O
N
A. Methadone
Beta Blockers from Urine
CN-015
100% organic wash
results in clean extracts
1
96%
100
3
90%
90
% Recovery
80
B
A
Sorbent:
Order No:
Condition:
Equilibrate:
Load:
Wash 1:
Wash 2:
Wash 3:
Elute:
Evaporate:
4
6
strata-X-C 30mg/1mL
8B-S029-TAK
1mL methanol
1mL water
1mL urine spiked with analytes; dilute
1:1 with phosphate buffer saline solution
pH 7; acidiﬁed with 2% phosphoric acid
1mL 0.1N HCI
1mL methanol, Dry for 1 min
1mL NH4OH/methanol water (2:50:48)
1mL 5% NH4OH/methanol
spike extract with external standard
(1µg/mL); dry down under nitrogen
and reconstitute with 200µL 20mM
KH2PO4 (pH 2.5)
60
50
40
2
0
2
SPE CONDITIONS
70
8
10
12
14
min
30
20
10
A
0
B
HPLC Column:
Order No:
Sample:
Mobile Phase:
Luna® 5µ C18(2), 150 x 4.6mm
00F-4252-E0
50µL of reconstituted extract
A: 20mM KH2PO4 (pH 2.5)
B: acetonitrile
Gradient: A/B (95:5) to (50:50) in 15 minutes
Flow rate: 1.5mL/min
Temperature: 25°C
Detector: UV @ 210nm
Peaks: 1. Pindolol (ext. std.)
2. Metoprolol
3. Propanolol
Chromatogram of Extracts:
A) Blank B) Spiked Sample
OH
NH
O
O
A. Metoprolol
NH
O
OH
B. Propanolol
PHENOMENEX • WEB: www.phenomenex.com
9
strata-X-C: Multimode Selectivity For High Recoveries
38000
36000
34000
32000
30000
ity strata-X-C exhibits strong π-π, polar
and hydrophobic secondary interactions.
THC from Urine
28000
24000
22000
These numerous retention mechanisms
20000
can be used to selectively extract analyt-
18000
es from an unknown mixture or develop
CN-001
26000
Peaks:
THC-COOH-d3 (IS)
THC-COOH (analyte)
16000
14000
sensitive SPE methods that may require
12000
detection on a mass spec.
10000
90
80
8000
6000
A
B
4000
2000
3
4
5
6
7
8
9
10
11
12 min
SPE CONDITIONS
Sorbent:
Order No:
Condition:
Equilibrate:
Load:
strata-X-C 60mg/3mL
8B-S029-UBJ
2mL methanol
2mL 0.1 N HCI
Base hydrolysis: 2mL urine spiked with
analyte and IS, add 100µL 10 N KOH.
Mix, vortex and hydrolyze for 20 min at
60°C. Cool and adjust pH to 3.5-4.0 (by
adding 200µL glacial acetic acid)
Wash 1: 2mL 0.1 N HCI
Wash 2: 2mL 0.1 N HCl / acetonitrile (70:30)
Dry for 4 min under vacuum. To further
remove water: add 200µL glacial acetic
acid, letting it percolate under gravity
for 30-40 sec. Dry sorbent for 1 min
under vacuum
Elute: 2mL 2% glacial acetic acid/acetonitrile
10
PHENOMENEX • WEB: www.phenomenex.com
99%
100
% Recovery
In addition to cation exchange selectiv-
70
60
50
40
30
20
10
Evaporate: under nitrogen and reconstitute with
30µL 10 mM imidazole/ethylacetate +
30µL BSTFA (1% TMCS). React at 70°C
for 20 min.
A
0
GC Column:
Order No:
Dimension:
Injection:
Carrier:
Oven program:
ZebronTM ZB-5
7EG-G002-11
15m x 0.25mm x 0.25µm
3µL splitless for 0.4 min at 270°C
Helium constant ﬂow at 1.8mL/min
160°C to 235°C at 20°C/min to 250°C
at 3°C/min to 340°C at 25°C/min
Detector: SIM mode (371, 374*, 473, 476*, 488,
and 491*); source=240°C; Transfer
line=300°C. * from d3 Internal
Standard (IS)
Chromatogram of Extracts:
A) Blank B) Spiked Sample
OH
OH
H
O
O
H
A. THC-COOH
Sulfa Drugs from Plasma
CN-011
99%
100
80
4
2
3
0
2
4
6
8
70
60
50
40
10
12
14
B
A
30
min
10
20
Wash 1:
Wash 2:
Elute:
Evaporate:
strata-X-C 30mg/1mL
8B-S029-TAK
1mL methanol
1mL water
1mL sample spiked with analytes and
IS (0.5µg/mL); dilute 1:1 with water
containing 2% phosphoric acid
1mL 0.1N HCI
1mL methanol, Dry 1 min under vacuum
1mL methanol
Spike 100µL of 1.0µg/mL Sulfanilamide
(IS) and dry down under slow stream of
N2 and reconstitute with 200µL
phosphate buffer.
A
0
SPE CONDITIONS
Sorbent:
Order No:
Condition:
Equilibrate:
Load:
HPLC Column:
Order No:
Sample:
Mobile Phase:
88%
90
High recoveries by strong secondary interactions
% Recovery
1
89%
Synergi Max-RP 4µ 150 x 4.6mm
00F-4337-E0
20µL of reconstituted extract
A: 20mM KH2PO4 (pH 2.5)
B: acetonitrile
Gradient: A/B (95:5) to (20:80) in 15 minutes
Flow rate: 1mL/min
Temperature: 25°C
Detector: UV@254nm
Peaks: 1. Sulfanilamide (IS)
2. Sulfathiazole
3. Sulfamethoxazole
4. Sulfaquinoxaline
Chromatogram of Extracts:
A) Blank B) Spiked Sample
B
C
TM
O
O
S
O
S
H2N
O
O
O
S
O
S
H2N
S
N
N
H
H2N
O
N
H
S
O
H2N
CH3
O
S
H N
N
H
S
N
N
B. Sulfamethoxazole
O
H
N
N
A. Sulfathiazole
O
S
O
N
N
N
H
N
H2N
N
N
H
S
O
S
H
N
O
S
N
H
N
O
NH2
S
O
NH2
S
O
O
N
H
CH3
NH2
S
O
C. Sulfaquinoxaline
O
CH3
PHENOMENEX • WEB: www.phenomenex.com
11
12
SIMPLE
• Consistent sample processing
eliminates variable extractions
• Deconditioning resistant
sorbents maintain selectivity
for high recoveries
• Versatile formats for high
throughput and large volume
cleanup
13
Consistent Sample Processing
Traditional SPE Sorbents
strata-X and strata-X-C are deconditioning resistant and will not lose
strata-X and strata-X-C
selectivity after the sorbent bed runs
Si
or during 96-well plate automation.
Si
OH
Si
OH
OH
Si
H20
H20
Si
Si
Si
Polymer
Polymer
Particle
SilicaSilica
Particle
DECONDITIONED AFTER SORBENT RUNS DRY
Si
14
PHENOMENEX • WEB: www.phenomenex.com
Si
Si
Si
Si
SiOH
OH
OH
Si
OH
SiSi
Si
Si
H20
H20
H20
H20
Si
MeOH
Si
MeOH
H20
MeOH
H20
OH
OH
H20
SiOH
MeOH
Si
Si
MeOH
H20
Si
Si
H20
cessing samples on a vacuum manifold
MeOH
becoming deconditioned when pro-
H20
sorbents, as a result of the sorbent
H20
eries, which occurs on traditional SPE
H20
H20
processing, preventing variable recov-
H20
resistant
H20
deconditioning
H20
H20
The
ability results in consistent sample
H20
dry.
Si
OH
OH
Si
Si
Si
REMAINS CONDITIONED AFTER SORBENT RUNS DRY
Si
Particle
SilicaSilica
Particle
Polymer
Polymer
Analyte
Recoveries
LowLow
Analyte
Recoveries
High
Analyte
Recoveries
High
Analyte
Recoveries
Formats for Simple Development
For cleanup that requires large sample
volumes or high-throughput methods
that require low elution volumes for
speed and sensitivity. strata-X and
strata-X-C are available in traditional,
high-throughput, and rapid extraction
formats for simple SPE automation and
method development.
High-Throughput
Rapid Extraction*
Available in strata-X only
*
Traditional Screening
Large Scale Cleanup
PHENOMENEX • WEB: www.phenomenex.com
15
16
VERSATILE
• Polymeric surface results in
simple cleanup, solvent switch
and analyte concentration
• Multimode selectivity for
streamlined method
development
• Wide ﬂexibility for all
SPE applications
17
Wide Flexibility for All SPE Applications
LIFE
SCIENCE
Desalting of Peptides
SELECTIVE ELUTION
91%
106%
104%
102%
PHENOMENEX • WEB: www.phenomenex.com
2
EQUILIBRATE
1mL water
3
100 90
2
EQUILIBRATE
1mL water
Sample Load
in 100mM NaCl
90 80
3
Sample Load
in 100mM NaCl
WASH
2 x 1mL water
80 70
4
WASH
2 x 1mL water
70 60
5
ELUTE BASIC PEPTIDES
acetonitrile/0.1% formic
acid in water (70:30) ELUTE NEUTRAL PEPTIDES
6
ELUTE NEUTRAL PEPTIDES
acetonitrile/water (70:30)
7
ELUTE ACIDIC PEPTIDES
acetonitrile/water (40:60)
106%
104%
102%
% Recovery
100%
60 50
20
10
0
5
7
20
10
0
4
6
50 40
40
30
18
CONDITION
1mL acetonitrile
CONDITION
1mL acetonitrile
91%
30
SELETIVE ELUTION
A. Bradykinin
B. Angiotensin I
C. Angiotensin II
D. Angiotensin III
E. HGRH
1
1
100
% Recovery
100%
A
A
B
B
C
C
D
D
E
E
ELUTE BASIC PEPTIDES
acetonitrile/0.1% formic
acid in water (70:30)
acetonitrile/water (70:30)
ELUTE ACIDIC PEPTIDES
acetonitrile/water (40:60)
Peptides from Serum
CN-010
2
3
1
Polar and Non-Polar Selectivity
100
99%
96%
90
80
A
B
C
% Recovery
LIFE
SCIENCE
70
60
50
40
SPE CONDITIONS
Sorbent:
Order No:
Condition:
Equilibrate:
Load:
strata-X 30mg/1mL
8B-S100-TAK
1mL methanol
1mL water
1mL porcine serum spiked with
analyte and IS (5µg/mL) and 20µL
phosphoric acid
Wash 1: 1mL 10% acetonitrile in 0.1% TFA
Elute: 1mL acetonitrile/water (80:20, v/v)
Evaporate: Dry down under slow stream of N2
and reconstitute with 300µL 0.1%
aqueous TFA
D
HPLC Column: Jupiter™ Proteo, 4µ, 150 x 4.6mm with
SecurityGuard™ C18 column 4 x 3.0mm
Order Nos: 00F-4396-E0 and AJ0-6074
Sample: 10µL of reconstituted extract
Mobile Phase: A: 0.1% TFA; B: acetonitrile/water (90:1)
with 0.1% TFA
Gradient: A/B (85:15) to A/B (40:60) in 25 min
Flow rate: 1mL/min
Temperature: 30°C
Detector: UV@214nm
Peaks: 1. Oxytocin
2. Angiotensin (IS)
3. Angiotensin II
Chromatogram of Extracts:
A) Spiked Sample B) Wash C) Blank D) 2nd Wash
30
20
10
0
A
B
A. Oxytocin
B. Angiotensin II
PHENOMENEX • WEB: www.phenomenex.com
19
Wide Flexibility for All SPE Applications
Environmental
Urea Pesticides in Water
CN-022
Polar and Non-Polar Selectivity
102%
108%
75%
99%
91%
A
B
C
D
E
100
90
2
3
4
5
80
6
% Recovery
1
70
60
50
40
B
A
30
20
10
0
2
4
6
8
10
12
14
16 min
0
SPE CONDITIONS
Sorbent:
Order No:
Condition:
Equilibrate:
Load:
Wash 1:
Elute:
strata-X 60mg/3mL
8B-S100-UBJ
2 mL dichloromethane
2mL acetonitrile; 2mL water
2mL spiked tap water
2mL water; Dry for 2 min
2 mL of acetonitrile/ dichloromethane
(1:1) add 20µg/mL of Linuron
(external standard, E.S)
Evaporate: under nitrogen and reconstitute
with 200µL water
20
PHENOMENEX • WEB: www.phenomenex.com
HPLC Column:
Order No:
Sample:
Mobile Phase:
Gradient:
Luna™ 5µ C18(2) 150 x 4.6 mm
00F-4252-E0
50µL of reconstituted water extract
A: water; B: acetonitrile
A/B (85:15) hold for 2 min to A/B (42:58)
in 13 min hold for 2 min
Flow Rate: 2mL/min
Temperature: 25° C
Detector: UV @ 214nm
Peaks: 1. Fenuron
2. Monuron
3. Forchlorfenuron
4. Diuron
5. Siduron
6. Linuron (E.S.)
Chromatogram of Extracts:
A) Blank B) Spiked Sample
A. Fenuron
B. Monuron
C. Forchlorfenuron
D. Diuron
E. Siduron
PAHs from Water
CN-021
Polar and Non-Polar Selectivity
92%
89%
82%
67%
81%
79%
A
B
C
D
E
F
100
90
5
1
3
2
4
80
6
% Recovery
Environmental
7
70
60
50
40
30
B
A
10.00
11.00
12.00
13.00
14.00
15.00
16.00
17.00
18.00
19.00
20.00
20
10
21.00 min
0
SPE CONDITIONS
Sorbent:
Order No:
Condition:
Equilibrate:
Load:
Wash 1:
Elute:
strata-X 60mg/3mL
8B-S100-UBJ
2 mL dichloromethane
2mL acetonitrile; 2mL water
10mL spiked tap water
2mL water; Dry for 2 min
2 x 2mL dichloromethane Add 100 µL of
20 µg/mL benzo[g.h,i] perylene
Evaporate: Blow down to dryness under N2, and
reconstitute with 100 µL dichloromethane
GC Column:
Order No:
Dimension:
Injection:
Carrier:
Oven program:
ZebronTM ZB-5
7HG-G002-11
30m x 0.25mm x 0.25µm
1µL splitless for 0.4 min at 280°C
Helium constant ﬂow at 1.1mL/min
120°C to 320°C at 10°C/min hold
for 2 min
Detector: MSD Scan mode (50 to 450 amu);
source= 240°C; transfer line=320° C
Peaks: 1. Fluoranthene 6. Benzo[a]pyrene
2. Pyrene
7. Benzo[g,h,i] perylene (E.S)
3. Benz[a]anthracene
4. Chrysene
5. Benzo[b]ﬂuoranthene
Chromatogram of Extracts:
A) Blank B) Spiked Sample
A. Fluoranthene
B. Pyrene
C. Benz[a]anthracene
D. Chrysene
E. Benzo[b]ﬂuoranthene
F. Benzo[a]pyrene
PHENOMENEX • WEB: www.phenomenex.com
21
Wide Flexibility for All SPE Applications
Food &
Beverage
Single Step Extraction of Acrylamide
2µg/mL acrylamide in 0.2g French fries;
UV detection at 210nm
2.922 - Acrylamide
Streamlined method
development
TN-007
100
>78%
≥84%
>91%
B
C
90
% Recovery
80
70
60
50
40
30
20
10
0
SPE CONDITIONS
Sorbent:
Order No:
Condition:
Equilibrate:
Load:
strata-X-C 200mg/3mL
8B-S029-FBJ
2 x 1mL methanol
2 x 1mL water
1mL homogenized supernatant;
Dry for 30 sec
Elute: 1mL water at a ﬂow rate of 0.5mL/min
Evaporate: remove excess water
22
PHENOMENEX • WEB: www.phenomenex.com
HPLC Column:
Order No:
Sample:
Mobile Phase:
Flow rate:
Temperature:
Detector:
SynergiTM Polar-RP® 150 x 3.0mm
00F-4336-Y0
10µL of extract
water / acetonitrile (94:6)
0.4mL/min
25°C
UV@210nm
A
A. Acrylamide 50ng/mL
B. Acrylamide 500ng/mL
C. Acrylamide 2000ng/mL
Barbiturates from Urine
CN-005
High recoveries by strong cation
exchange retention mechanism
101%
103%
100%
A
B
C
100
1
90
80
2
% Recovery
Toxicology
4
3
70
60
50
40
B
30
A
20
10
0
2
4
6
8
10
11
12
min
0
SPE CONDITIONS
Sorbent:
Order No:
Condition:
Equilibrate:
Load:
Wash 1:
Wash 2:
Elute:
Evaporate:
strata-X-C 60mg/3mL
8B-S029-UBJ
2mL methanol
2mL water
2mL human urine spiked with analytes
and IS (0.5µg/mL), dilute 1:1 with water
2mL 5% methanol in water
2mL 10% methanol in 2% acetic acid
and dry for 1min
2mL 35% methanol/2% NH4OH
dry down under slow stream of N2 and
reconstitute in 300µL mobile phase
Phenobarbital
Phenobarbital
HPLC Column:
Order No:
Sample:
Mobile Phase:
SynergiTM Max-RP 4µ 150 x 4.6mm
00F-4337-E0
50µL of reconstituted extract
A: 20mM KH2PO4 ( pH 7.0)
B: acetonitrile
Gradient: A/B (80:20) hold 3 min. to (50:50)
in 12 minutes
Phenobarbital
Flow rate: 1.0mL/min
O
Temperature: 25°C O
NH
Detector: UV @ 214nm
NH
Peaks: 1. Phenobarbital
3. Amobarbital
2. Butalbital O
4. Secobarbitol (I.S.)
Chromatogram of Extracts:
A) Blank B) Spiked Sample
Amobarbital
O
O
O
O
O
NH
NH
NH
NH
O
O
A. Phenobarbital
Amobarbital
Amobarbital
Butalbital
O
NH
O
O
O
NH
NH
O
B. Butalbital
O
O
NH
NH
NH
O
O
C. Amobarbital
Secobarbital • WEB: www.phenomenex.com
PHENOMENEX
NH
O
23
strata-X and strata-X-C Ordering Information
Rapid Screening
ORDER NO.
DIMENSIONS
00M-S033-B0-CB
strata-X on-line extraction cartridge,
25µm, 20 x 2.0mm
UNIT/BOX
ea
CH0-5845
Cartridge holder, 20mm
ea
PRICE
Traditional Cleanup
1mL (100/box)
Phase
24
3mL (50/box)
6mL (30/box)
30mg
60mg
200mg
500mg
100mg
200mg
500mg
strata-X
8B-S100-TAK
8B-S100-UBJ
8B-S100-FBJ
8B-S100-HBJ
8B-S100-ECH
8B-S100-FCH
8B-S100-HCH
strata-X-C
8B-S029-TAK
8B-S029-UBJ
8B-S029-FBJ
8B-S029-HBJ
8B-S029-ECH
8B-S029-FCH
8B-S029-HCH
PHENOMENEX • WEB: www.phenomenex.com
High-Throughput (2/box)
Phase
strata-X
strata-X-C
5mg
10mg
30mg
60mg
8E-S100-NGB
8E-S100-AGB
8E-S100-TGB
8E-S100-UGB
—
8E-S029-AGB
8E-S029-TGB
8E-S029-UGB
Large Sample Cleanup
12mL (20/box)
Phase
strata-X
strata-X-C
20mL (20/box)
100mg
500mg
1g
1g
—
8B-S100-HDG
8B-S100-JDG
8B-S100-JEG
8B-S029-EDG
8B-S029-HDG
8B-S029-JDG
—
PHENOMENEX • WEB: www.phenomenex.com
25
SPE Accessories Ordering Information
96-Well Plate Accessories
ORDER NO.
DESCRIPTION
UNIT
Manifold
AH0-7284
96-Well Plate Manifold, Acrylic
ea
Sealing Mats
AH0-7195
Pierceable Sealing Mats, 96 Square Well
50/pk
AH0-7362
Sealing Tape Pad
10/pk
AH0-7192
0.35mL/well 96 Square Well Collection Plate
50/pk
AH0-7193
1mL/well 96 Square Well Collection Plate
50/pk
AH0-7194
2mL/well 96 Square Well Collection Plate
50/pk
AH0-7408
Solvent Waste Reservoir Tray
25/pk
Collection Plates
Vacuum Manifolds*
Order No.
Description
Unit
24-Position Vacuum Manifold
AH0-6024
Complete Assembly for 1,3, 6mL Tubes
ea
12-Position Vacuum Manifold
AH0-6023
Complete Assembly for 1, 3, 6mL Tubes
ea
10-Position Vacuum Manifold
AH0-7502
Tall-Boy Vacuum Manifold
Complete Assembly for Giga Tubes
* Replacement parts available contact your local Phenomenex technical consultant or distributor.
26
PHENOMENEX • WEB: www.phenomenex.com
ea
Price
PRICE
Technical
Notes Available
Contact Phenomenex or your Local
Phenomenex Distributor and Request
a Technical Note Today.
X
• Extraction of Phenols from Water using strata-X (TN-001)
• Extraction of Nitroanilines from Water using strata-X (TN-003)
• Extraction of Acidic, Basic, and Neutral Compounds using
strata-X (TN-004)
• TCAs Extracted from Serum using strata-X (TN-006)
• Fast Extraction of Acyclovir from Plasma using strata-X
On-line Cartridge (TN-009)
X-C
• Rapid Removal of Acrylamide from French Fries using
strata-X-C (TN-007)
• Basic Drugs from Biological Matrices on strata-X-C (TN-008)
• Extraction of Sulfa Drugs from Plasma using strata-X-C
(TN-010)
Luna™, Zebron™, Jupiter™, SecurityGuard™ Synergi™, and Strata™ are trademarks of Phenomenex. SPE Applications shown
may not be representative of all SPE applications. © 2004 Phenomenex. All rights reserved.
PHENOMENEX • WEB: www.phenomenex.com
27
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