ACE UHPLC and HPLC Columns
Nitrosamines European Toy Standard Method by LC-MS/MS
XIC of +MRM (34 pairs): 101.200/55.300 amu Expected RT: 8.7 from Sample 14 (100 std) of 30092014.wiff (Heated Nebulizer) Max. 1.0e6 cps.
4
8.31
1
2
3
7
6
5
12
13
9
10
11
8
14
10
2 4 12 14 18 20 22 24 26 28 30
Time, min
Non-Steroidal Anti-Inflammatory Drugs (II)
Conditions Analytes
Column: ACE Excel 5 SuperC18
Dimensions: 150 x 4.6 mm
Part Number: EXL -1211-1546U
Mobile Phase: A: 0.1% formic acid in H2O
B: 0.1% formic acid in MeCN
Gradient: Time (mins) %B
0 20
20 70
25 70
36 20
Flow Rate: 1 mL/min
Injection: 10 μL
Temperature: 40 °C
Detection: UV, 254 nm
5
4
3
5 10 15 20 25
Time - Minutes
Application #AN1220
1. Aspirin
2. Phenacetin
3. Sulindac
4. Tolmetin
5. Naproxen
6. Nimesulide
7. Flurbiprofen
8. Diclofenac
9. Phenylbutazone
10. Meclofenamic acid
min
mAU
mAU
1000
1000
800
800
600
600
400
400
200
200
0
0
9
7
6 8
10
2
1
4.6e6
4.6e6
4.4e6
4.4e6
4.2e6
4.2e6
4.0e6
4.0e6
3.8e6
3.8e6
3.6e6
3.6e6
3.4e6
3.4e6
3.2e6
3.2e6
3.0e6
3.0e6
2.8e6
2.8e6
2.6e6
2.6e6
2.4e6
2.4e6
2.2e6
2.2e6
2.0e6
2.0e6
1.8e6
1.8e6
1.6e6
1.6e6
1.4e6
1.4e6
1.2e6
1.2e6
1.0e6
1.0e6
8.0e5
8.0e5
6.0e5
6.0e5
4.0e5
4.0e5
2.0e5
2.0e5
0.0
Intensity, cps
Non-Steroidal Anti-Inflammatory Drugs (I)
www.ace-hplc.com | +44 (0) 1224 704 554 | info@ace-hplc.com 107
Conditions Analytes
Reproduced with permission of LGC Limited, UK
3
1
2
4
5
6
7
8
9
11
12
13
14
0.0 2 4 6 8 10 12 14 16 18 20 22 24 26 28
Time - Minutes
Intensity, cps
Application #AN1110
Column: ACE Excel 2 C18-PFP
Dimensions: 150 x 3.0 mm
Part Number: EXL -1010-1503U
Mobile Phase: A: 0.1% formic acid in H2O
B: 0.1% formic acid in MeOH
Gradient: Time (mins) %B
0.0 5
1.0 5
10.0 65
14.0 65
15.0 90
20.0 90
21.0 5
30.0 5
Flow Rate: 0.35 mL/min
Injection: 20 μL
Temperature: 40 °C
Sample
Temperature: 4 °C
Detection: Applied Biosystems 4000 Q-Trap MS
Source: APCI (positive mode)
Collision energy: 10-30 V
Source temperature: 300 °C
1. NDELA
(m/z 135.2 74.2, 135.2 104.2)
2. NDMA
(m/z 74.9 43.2, 74.9 58.2)
3. Nmorph
(m/z 117.1 86.3, 117.1 73.3)
4. Npyrr
(m/z 101.2 55.3, 101.2 59.2)
5. NMEA
(m/z 89.2 61.1, 89.2 43.3)
6. NDEA
(m/z 103.1 75.2, 103.1 47.2)
7. NPIP
(m/z 115.1 69.1, 115.1 41.2)
8. NDnPA
(m/z 131.2 89.2, 131.2 43.3)
9. NdiPA
(m/z 131.2 89.2, 131.2 43.3)
10. NMPhA
(m/z 137.2 107.2, 137.2 66.1)
11. NEPhA
(m/z 151.1 77.1, 151.1 95.3)
12. NDiBA
(m/z 159.3 57.2, 159.3 103.2)
13. NDnBA
(m/z 159.3 103.2, 159.3 57.2)
14. NDBzA
(m/z 227.2 91.1, 227.2 181.2)
European Union EN 71-12 Safety of Toys:
N-Nitrosamines and N-nitrosatable substances e.g.
Analysis of nitrosamines in balloon extracts
Conditions Analytes
2
3
4
Time - Minutes
Application #AN1210
Column: ACE 3 C18-AR
Dimensions: 150 x 4.6 mm
Part Number: ACE-119-1546
Mobile Phase: A: 0.1% formic acid in H2O
B: 0.1% formic acid in MeOH
Gradient: Time (mins) %B
0 52
28 74
33 74
38 52
48 52
Flow Rate: 1 mL/min
Injection: 5 μL
Temperature: 40 °C
Detection: UV, 254 nm
1. Bendroflumethiazide
2. Ketoprofen
3. Naproxen
4. Sulindac
5. Ibuprofen
6. Diclofenac
7. Indomethacin
8. Meclofenamic acid
9. Mefenamic acid
5
6
7
8 9
10 min
mAU
mAU
1
0 5 10 15 20 25 30