219 / 413
•
21
•
2008 vol. 1
Clinical/Forensics
Allure® PFP Propyl Columns (USP L43)
Excellent Columns for LC/MS and ELSD
Physical Characteristics:
5µm Column, 2.1mm
cat. #
price
50mm
9169552
50mm (with Trident Inlet Fitting)
9169552-700
particle size: 3µm or
5µm, spherical
pore size: 60Å
carbon load: 17%
endcap: fully endcapped
pH range: 2.5 to 7.5
temperature limit: 80°C
Allure
®
PFP Propyl Guard Cartridges qty.
cat. #
price
10 x 2.1mm
3-pk.
916950212
10 x 4.0mm
3-pk.
916950210
20 x 2.1mm
2-pk.
916950222
20 x 4.0mm
2-pk.
916950220
Trident Direct Guard Cartridge System
*The standard PEEK™ tip in Trident Direct systems is compatible with Parker
®
, Upchurch
Scientific
®
, Valco
™
, and other CPI-style fittings. To use Trident Direct systems with Waters-style end
fittings, replace the tip with cat.# 25088.
Description
qty.
cat.#
price
High-pressure filter
ea.
25082
10mm guard cartridge holder without filter
ea.
25083
10mm guard cartridge holder with filter
ea.
25084
20mm guard cartridge holder without filter
ea.
25085
20mm guard cartridge holder with filter
ea.
25086
Solvent
Compound
CAS# Code Conc.
cat.#
(ea.) price
alprazolam 28981-97-7 PTM 1,000 34042
bromazepam 1812-30-2 PTM 1,000 34043
chlordiazepoxide 438-41-5 PTM 1,000 34044
clobazam 22316-47-8 PTM 1,000 34045
clonazepam 1622-61-3 PTM 1,000 34046
diazepam
439-14-5 PTM 1,000 34047
flunitrazepam 1622-62-4 PTM 1,000 34049
flurazepam 1172-18-5 PTM 1,000 34050
lorazepam 846-49-1 PTM 1,000 34051
nitrazepam 146-22-5 PTM 1,000 34053
oxazepam 604-75-1 PTM 1,000 34054
prazepam 2955-38-6 PTM 1,000 34055
temazepam 896-50-4 PTM 1,000 34056
triazolam 28911-01-5 PTM 1,000 34057
Exempted Drug of Abuse Reference
Materials: Benzodiazepines
Concentration is µg/mL. Volume is 1mL/ampul.
The Allure® PFP Propyl stationary phase provides baseline resolution for
compounds sharing the same precursor ion, such as nordiazepam and
medazepam. The ability to chromatographically separate compounds with
similar spectra allows this method to be adapted for single stage MS, however,
the LOQ values would be affected. Tandem MS is advantageous since two
MRM transitions are collected, allowing quantification and confirmation to
be accomplished in a single run, without loss of sensitivity.
Conclusion
Themethod presented here provides significant advantages over other techniques
for benzodiazepine analysis: simple sample preparation, fast analysis time (less
than 10 minutes), LOQs of 0.10-10ng/mL in matrix, and quantification and
confirmation in a single run. Further, using the retentive Allure® PFP Propyl
column eliminates coelution of matrix peaks with target compounds and
assures full chromatographic resolution of analytes with shared precursor ions.
Acknowlegement
We sincerely thank Andre Schreiber of Applied Biosystems and Houssain El Aribi and John Gibbons of
MDS Sciex for supplying the method and data.
References
Schreiber, Andre PhD, El Arbi, Houssain and Gibbons, John. 2007. A Fast and Sensitive LC/MS/MS
Method for the Quantitation and Confirmation of 30 Benzodiazepines and Nonbenzodiazepine
Hypnotics in Forensic Urine Samples. Applied Biosystems MDS Sciex.
Compound Name
Retention Time
Precursor Ion
MRM 1
MRM 2
DP
CE
CE
LOQ
(min.)
(amu)
(amu)
(amu)
(MRM 1)
(MRM 2)
(ng/mL)
7-aminonitrazepam
3.2
252.1
121.1
94.0
51
35
53
1.0
7-aminoclonazepam
3.3
286.1
121.0
222.2
46
41
35
0.5
7-aminoflunitrazepam
3.8
284.1
135.1
226.0
51
39
49
0.5
Bromazepam
3.8
316.0/318.0
182.1
182.1
51
45
45
5.0
α
-hydroxyalprazolam
4.1
325.1
297.2
204.9
51
31
59
2.0
α
-hydroxytriazolam
4.1
359.0
239.2
176.0
61
63
37
5.0
Oxazepam
4.2
287.0
241.1
268.9
41
27
19
10.0
Lorazepam
4.3
321.0/323.1
275.0
277.0
41
31
27
5.0
Estazolam
4.4
295.0
205.0
267.1
51
53
31
2.0
Zaleplon
4.4
306.2
236.3
264.2
56
35
27
0.5
2-hydroxyethylflurazepam
4.5
333.1
211.2
109.0
56
51
41
1.0
Desmethylflunitrazepam
4.5
300.1
254.2
198.2
56
35
51
2.0
Nitrazepam
4.6
282.0
236.1
180.2
71
35
51
2.0
Clonazepam
4.7
316.0
270.2
214.0
56
41
51
2.0
Desalkylflurazepam
4.7
289.1
140.1
226.1
71
41
39
2.0
Temazepam
4.7
301.1/303.1
255.1
257.2
35
30
30
5.0
Triazolam
4.7
343.0
238.9
314.9
61
53
37
1.0
Alprazolam
4.8
309.1
205.1
281.1
56
53
35
1.0
Lormetazepam
4.8
335.0/337.1
289.0
291.1
41
29
29
2.0
Clobazam
4.9
301.1
259.1
224.3
46
29
47
1.0
Flunitrazepam
5.0
314.0
268.1
239.1
56
35
49
1.0
Nordiazepam
5.0
271.1
140.2
164.9
46
37
35
2.0
Zolpiclone
5.4
389.1
244.8
217.0
16
25
41
1.0
D5-Diazepam
5.4
290.1
198.2
-
55
41
-
Diazepam
5.5
285.0
193.2
154.1
55
41
37
1.0
Chlordiazepoxide
6.0
300.1
227.1
283.2
36
31
21
5.0
Prazepam
6.1
325.1
271.1
140.0
81
31
53
2.0
Zolpidem
7.4
308.1
235.1
236.1
56
39
35
0.2
Midazolam
7.9
326.1
291.3
222.0
56
33
63
0.5
Flurazepam
8.5
388.2
315.1
317.1
36
27
27
0.1
Medazepam
9.0
271.0
91.1
207.3
46
41
39
2.0
D3-Doxepine
9.1
283.0
107.1
-
41
35
-
Table I
MRM Transitions, retention times, and LOQ values.
Bar color indicates shared precursor ions. Note compounds with shared precursor ions are baseline resolved on the Allure
®
PFP Propyl column,
as shown by retention time comparison.
Data courtesy of Applied Biosystems MDS Sciex.
PTM=purge & trap grade methanol