Page 32 - Application Handbook - Liquid Chromatography

Application No.L476
News

n Rapid Analysis of 2,4-DNPH-Derivatized Aldehydes
and Ketones mV (×10)
Next, we investigated the use of the Shim-pack XR-ODS n Peaks
(75 mm × 4.6 mm, 2.2 µm) column to shorten the run 1. Formaldehyde

2. Acetaldehyde
time. Fig. 3 shows the resulting chromatogram, and 5.0 3. Acetone

Table 3 shows the analytical conditions used. The 1 4. Acrolein

5. Propionaldehyde
detection limit of formaldehyde was determined to be 4.0 6. Crotonaldehyde
7. 2-Butanone
12 pg, and the limit of quantitation, 37 pg. Even with 8. Methacrolein
9. n-Butyraldehyde
the analysis time shortened by half, from 30 minutes to 3.0 2 4 10. Benzaldehyde
15 minutes, the chromatogram showed no adverse 3 5 11. Valeraldehyde
12. m-Tolualdehyde
effects on resolution or peak shape. 2.0 6 8 13. Hexanaldehyde
7 9
10 11
1.0 12 13
2
7 11 13
Table 3 Analytical Conditions 0.0
Column : Shim-pack XR-ODS (75 mm L. × 4.6 mm I.D., 2.2 µm)
Mobile Phase : A : Water/THF = 8/2 0.0 2.5 5.0 7.5 10.0 12.5 min
B : Acetonitrile
Time Program : B Conc. 20 % → 60 % (15 min) → 20 % (15-17 min)
Flowrate : 1.5 mL/min Fig. 3 Chromatogram of Standard Sample
Injection Volume : 10 µL (each at 1.0 mg/L as carbonyl compounds)
Column Temp. : 40 °C
Detection : UV 360 nm
n Linearity in Rapid Analysis
Calibration curves were also generated using the Shim- ×10 5
pack XR-ODS for high-speed analysis of solutions at 7 Formaldehyde
concentrations ranging from 0.03 to 3 mg/L (10 µL
injected) prepared by stepwise dilution of the stock 6 2-Butanone R =0.99996
2
standard solutions of the thirteen 2,4-DNPH-derivatized Hexanaldehyde
aldehydes and ketones. Fig. 4 shows the calibration 5
curves for formaldehyde, 2-butanone, and
hexanaldehyde. These also showed excellent linearity 4 R =0.99997
2
2
with R values greater than 0.9999. The area %RSD Peak Area
values at a concentration of 1.0 mg/L for all 3
components were within 1 %, as shown in Table 4.
2
R =0.99995
2
1
Table 4 Repeatability of Peak Area (n=3)
Area %RSD Area %RSD 0
Formaldehyde 0.255 Methacrolein 0.229 0 1 2 3
Acetaldehyde 0.139 n-Butyraldehyde 0.333 Concentration (mg/L)
Acetone 0.139 Benzaldehyde 0.247
Acrolein 0.226 Valeraldehyde 0.101 Fig. 4 Linearity
Propionaldehyde 0.171 m-Tolualdehyde 0.917
Crotonaldehyde 0.423 Hexanaldehyde 0.579
2-Butanone 0.333

First Edition: Nov. 2014

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