267 / 413
Figure 2
Derivatized hormones show excellent resolution and more symmetrical peak shapes than underivatized
hormones.
•
13
•
2007 vol. 3
For the derivatization proce-
dure used in this analysis,
see Knapp’s
Handbook of
Analytical Derivatization
Reactions
, page 482.
Rxi™-1ms Columns (fused silica)
(Crossbond
®
100% dimethyl polysiloxane)
ID df (µm)
temp. limits
length cat. #
price
0.25mm 0.25 -60 to 330/350°C 30-Meter 13323
$450
GC_PH00872
1. androsterone
2. dehydroepiandrosterone (DHEA)
3. 17-
α
-estradiol
4. estrone
5. 17-
β
-estradiol
6. testosterone
7. derivatization by-product
Low bleed at 300+°C!
20.0
2
1
4
3
5
6
15.0
25.0
Column:
Rxi™-1ms 30m, 0.25mm ID, 0.25µm (cat. # 13323)
Inj.:
1.0µL splitless (hold 0.5min.), 3.5mm single
gooseneck inlet liner (cat.# 20961)
Inj. temp.:
250°C
Carrier gas:
helium, constant flow
Flow rate:
1mL/min.
Oven temp.:
100°C to 320°C @ 10°C/min. (hold for 10 min.)
Det.:
MS: Shimadzu 17A with QP5000
Transfer line temp.: 280°C
Scan range:
40-700amu
Ionization:
EI
Mode:
Scan
GC_PH00923
min.
Sample: Sex hormones, 100µg/mL each, underivatized
Sample: 100µg/mL each hormone in methanol
or ethanol; compounds derivatized using 2%
methoxylamine HCl (CH
3
ONH
2
) in pyridine
A) Derivatized hormones
B) Underivatized hormones
Splitless Liners for Shimadzu GCs
**Nominal ID at syringe needle expulsion point.