有这里有检测的标准方法,为检测公司SOP的检测方法,不知能不能帮到你。
(1), Method for SIM Positive
HPLC-DAD: Agilent 1200
API-ES: Agilent 6130
Column: XDB-C18 narrow-bore column, 5um, 150*2.1mm
Guard Column: XDB-C18 narrow-bore guard column, 2.1*12.5mm, 5um
Flow rate: 0.3mL /min
Injection volume: 10uL
Column temperature: 30℃
Mobile phase:
A: 0.01M ammonium acetate buffer, PH=3.6
B: Acetonitrile
Min A (%) B(%)
0 60 40
15 40 60
25 20 80
28 20 80
30 60 40
32 60 40
Run time: 32min
Post time: 5min
MS parameters:
Ionization: Atmospheric Pressure Ionization-Electrospray (API-ES)
Spray pressure: 40 psi
Drying gas (nitrogen) temperature: 350℃
Drying gas flow: 12L/min
Fragmentor: 120V
Peakwidth: 0.1min
MS mode: SIM Positive (refer to Appendix A)
(2), Method for SIM Negative
HPLC-DAD: Agilent 1200
API-ES: Agilent 6130
Column: XDB-C18 narrow-bore column, 5um, 150*2.1mm
Guard Column: XDB-C18 narrow-bore guard column, 2.1*12.5mm, 5um
Flow rate: 0.3mL /min
Injection volume: 10uL
Column temperature: 30℃
Mobile phase:
A: 0.01M ammonium acetate buffer, PH=3.6
B: Acetonitrile
Min A (%) B(%)
0 90 10
3 70 30
8 50 50
15 30 70
15.1 5 95
20 5 95
Run time: 25min
Post time: 10min
MS parameters:
Ionization: Atmospheric Pressure Ionization-Electrospray (API-ES)
Spray pressure: 40 psi
Drying gas (nitrogen) temperature: 350℃
Drying gas flow: 12L/min
Fragmentor: 120V
Peakwidth: 0.9min
Cycle Time: 1.02sec/cycle
MS mode: SIM Negative (refer to Appendix A)
Appendix A – Retention time and m/z used in qualification and quantitation of colorants
Dye RT/min SIM ion (+ve) SIM ion (-ve)
Disperse Blue 1 2.596 268 --
Disperse Blue 106 9.526 336 --
Disperse Blue 124 17.479 378 --
Disperse Orange 3 11.231 243 --
Disperse Orange 37 22.779 392 --
Solvent Yellow 1 9.760 198 --
Solvent Yellow 2 21.208 226 --
Solvent Yellow 3 16.555 226 --
Basic Red 9 1.315 288 --
Basic Violet 1 8.881 358 --
Basic Violet 3 11.510 372 --
Disperse Blue 3 4.759 297 --
Disperse Yellow 3 11.098 270 --
Disperse Red 1 3.930 315 --
Acid Red 26 7.415 -- 435
Acid Violet 49 2.236 712 --
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求HPLC-DAD-MS技术测定组织中分散染料的方法