Determination of Nitrosamine


Instruction

This application note describes the GS-Tek column separates eight nitrosamines according to EPA 521&607. The standard mix of eight compounds ,such as N-nitrosodimethylamine (NDMA), N-nitrosomethylethylamine(NMEA), N-nitrosodiethylamine(NDEA), N-nitroso di-n-propylamine (NDPA), N-nitroso di-n-butylamine(NDBA), N-nitrosopiperidine(NPIP), N-nitrosopyrrolidine (NPYR) and N-nitrosodiphenylamine (NDPhA) was analyzed.

Comparing with Agilent CP-Wax 51 column, our GsBP-Wax-AQ column provides a higher resolution result, especially for a critical pair N-nitroso di-n-butylamine and N-nitrosopiperidine,shown as Figure 1&2. For some customers, they want to use 5MS, 35MS or 624 column for the separation,the resolution could be improved by adjusting the temperature program,chromatographic conditions appear above each figure.

Applicaion 1,

Column: GsBP-Wax-AQ, 30m x 0.25mm x 0.25um (PN: 2625-3002)
Carrier gas: @12.2psi
Oven: 40℃ -10℃ /min- 240℃
Split: 60ml/min
Inject volume: 0.1ul

nitrosamine-1

Figure 1.Chromatogram of nitrosamines on a GsBP-Wax-AQ column

 

nitrosamine-2

 

Figure 2.Chromatogram of nitrosamines on an Agilent CP-Wax 51 for Amines column

Table1. Peak Identification

Peak Name RT(min) K Resolution
1 N-nitrosodimethylamine(NDMA) 3.96 2.88
2 N-nitrosomethylethylamine(NMEA) 4.46 3.37
3 N-nitrosodiethylamine(NDEA) 4.78 3.68 10.59
4 N-nitrosodi-n-propylamine(NDPA) 6.42 5.29
5 N-nitrosodi-n-butylamine(NDBA) 8.61 7.44
6 N-nitrosopiperidine(NPIP) 8.9 7.72 12.62
7 N-nitrosopyrrolidine(NPYR) 9.33 8.14
8 Impuritiy 12.15 10.9
9 N-nitrosodiphenylamine(NDPhA) 17.55 16.2

 

Application 2,

Colunm: GsBP-5MS, 30m x 0.25mm x 0.25um (PN: 1525-3002)
Carrier gas@12.2psi
Oven: 60℃ -10℃ /min- 240℃ ( 2min)
Split: 60ml/min
Inject volume: 0.1ul

nitrosamine-3

 

Figure 3.Chromatogram of nitrosamines on a GsBP-5MS column

Table2. Peak Identification

Peak Name RT K Resolution
1 N-Nitrosodimethylamine(NDMA) 1.79 0.71
2 N-Nitrosomethylethylamine(NMEA) 2.34 1.25
3 N-Nitrosodiethylamine(NDEA) 3.02 1.89
4 N-Nitrosodi-n-propylamine(NDPA) 5.18 3.96
5 N-Nitrosopyrrolidine(NPYR) 5.28 4.06 4.15
6 N-Nitrosopiperidine(NPIP) 5.82 4.57
7 N-Nitrosodi-n-butylamine(NDBA) 8.11 6.77
8 N-Nitrosodiphenylamine(NDPhA) 12.97 11.4

 

Application 3,

Column: GsBP-35MS, 30m x 0.25mm x 0.25um (PN: 3525-3002)
Carrier gas@12.2psi
Oven: 60℃ -10℃ /min- 240℃
Split: 60ml/min
Inject volume: 0.1ul

nitrosamine-4Figure 4.Chromatogram of nitrosamines on a GsBP-35MS column

Table 3. Peak Identification

Peak Name MeasRetTime K Resolution
1 N-Nitrosodimethylamine 2.07 0.93
2 N-Nitrosomethylethylamine(NMEA) 2.67 1.5
3 N-Nitrosodiethylamine(NDEA) 3.31 2.09
4 N-Nitrosopyrrolidine(NPYR) 5.36 4.01
5 N-Nitrosodi-n-propylamine(NDPA) 6.42 5
6 N-Nitrosopiperidine(NPIP) 6.79 5.34 11.3
7 N-Nitrosodi-n-butylamine(NDBA) 7.93 6.41
8 N-Nitrosodiphenylamine(NDPhA) 13.86 11.94

Application 4,

Column: GsBP-624, 30m x 0.25mm x 1.40um (PN: 6525-3014)
Carrier gas@12.2psi
Oven: 60℃ -10℃ /min- 240℃
Split: 60ml/min
Inject volume: 0.1ul

nitrosamine-5

 

Figure 5.Chromatogram of nitrosamines on a GsBP-624 column

Table4. Peak Identification

Peak MeasRetTime K Resolution
1 N-Nitrosodimethylamine(NDMA) 4.89 3.45
2 N-Nitrosomethylethylamine(NMEA) 6.32 4.75
3 N-Nitrosodiethylamine(NDEA) 7.59 5.91
4 N-Nitrosopyrrolidine(NPYR) 10.71 8.75
5 N-Nitrosodi-n-propylamine(NDPA) 11.07 9.08 11.13
6 N-Nitrosopiperidine(NPIP) 11.67 9.62
7 N-Nitrosodi-n-butylamine(NDBA) 13.89 11.64
8 N-Nitrosodiphenylamine(NDPhA) 19.19 16.47
9 Impuritiy 19.37 16.63 4.74

 

GsBP-Wax-AQ, 30m x 0.25mm x 0.25um (PN: 2625-3002)
GsBP-624, 30m x 0.25mm x 1.40um (PN: 6525-3014)
GsBP-35MS, 30m x 0.25mm x 0.25um (PN: 3525-3002)
GsBP-5MS, 30m x 0.25mm x 0.25um (PN: 1525-3002)

Author: Zoe Wang, Zack Ji