lc/ms/ms一斉分析法の検討 - thermo fisher scientificはじめに...
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LC/MS/MS
LC-MS29 10 mg/L 0.2% EDTA 10
mg/L 0.2% EDTA
A p
p lic
a tio
n N
o te
L C
M S
1 3
0 0
UltiMate™ 3000
Thermo Scientific
Acclaim™ RSLC 120 C18 2.2 µm 150 x 2.1 mm Part No: 071399
A 0.1% B 5%B0min→95%B10min→95%B14min
→5%B14.1min to 20min
0.2 mL/min
MS Thermo Scientific
Ar1.0 mTorr
1SRM Timed SRM
No Precursor m/z
Product m/z
CE eV
Start min
Stop min
1 + 231 156 12 5.51 7.01 2 + 163 88 10 6.55 8.05 3 + 279 264 20 7.88 9.38 4 + 295 217 20 8.09 9.59 5 + 190 163 24 8.85 10.35 6 + 224 41 13 9.39 10.89 7 + 241 88 14 9.58 11.08 8 + 222 165 14 9.82 11.32 9 + 295 280 19 9.86 11.36 10 + 355 88 14 10.01 11.51 11 + 311 125 40 10.03 11.53 12 - 239 132 28 10.09 11.59 13 + 202 145 12 10.10 11.60 14 + 408 182 22 10.78 12.28
15 + 411 149 22 10.85 12.35
16 + 233 72 20 10.86 12.36 17 + 404 372 15 10.91 12.41 18 + 263 231 25 10.98 12.48 19 2,4-D - 219 161 15 11.08 12.58 20 + 233 137 20 11.29 12.79 21 - 254 196 13 11.51 13.01 22 + 269 151 14 11.54 13.04 23 - 213 141 18 11.66 13.16 24 - 435 330 16 11.85 13.35 25 + 398 314 12 11.90 13.40 26 + 435 182 22 11.97 13.47 27 + 330 245 16 12.05 13.55 28 + 334 139 22 12.29 13.79 29 + 279 169 20 12.40 13.90
2SRM 1
20 % 1/100 1 /1000 .005 µg/L CV%=8.3%1/1000.01 µg/L 0.01 µg/L 5.4%
2
1/100 µg/L
RT min
µg/L R2
%
2 6.25 0.005-5 0.9998 0.05 1.6 NF 0.106 106% 0.3 7.31 0.005-5 0.9978 0.05 1.2 NF 0.097 97% 0.01 8.63 0.005-5 0.9996 0.01 3.0 NF 0.099 99% 0.01 8.86 0.005-5 0.9996 0.01 1.9 0.099 99% 0.8 9.61 0.005-5 0.9986 0.05 1.1 NF 0.101 101% 0.5 10.15 0.005-5 0.9994 0.05 4.6 NF 0.092 92% 0.2 10.33 0.005-5 0.9946 0.05 3.7 NF 0.086 86% 0.05 10.58 0.005-5 0.9982 0.05 1.1 NF 0.105 105% 0.01 10.62 0.005-5 0.9987 0.01 5.4 NF 0.105 105% 0.8 10.79 0.005-5 0.9993 0.05 3.8 NF 0.100 100% 0.01 10.79 0.005-5 0.9991 0.01 3.3 NF 0.100 100% 2 10.78 0.005-1 0.9954 0.05 1.8 0.098 98% 0.5 10.85 0.005-5 0.9969 0.05 1.5 NF 0.104 104% 0.3 11.53 0.005-5 0.9989 0.05 2.7 NF 0.097 97% 4 11.60 0.005-1 0.9978 0.05 2.1 NF 0.100 100% 0.3 11.61 0.005-1 0.9961 0.05 2.1 NF 0.098 98% 5 11.68 0.005-5 0.9966 0.05 4.3 NF 0.102 102% 0.01 11.74 0.005-5 0.9993 0.01 2.7 NF 0.099 99% 2,4-D 0.3 11.76 0.005-5 0.9994 0.05 3.9 NF 0.091 91% 3 12.05 0.005-5 0.9995 0.05 1.8 NF 0.100 100% 0.06 12.20 0.01-5 0.9975 0.05 8.8 NF 0.088 88% 8 12.29 0.005-5 0.9990 0.05 1.0 NF 0.103 103% 0.05 12.37 0.005-5 0.9992 0.05 1.8 NF 0.094 94% 0.005 12.61 0.005-1 0.9991 0.005 8.3 NF 0.098 98% 1 12.65 0.005-5 0.9974 0.05 2.5 NF 0.099 99% 3 12.71 0.005-5 0.9986 0.05 1.3 NF 0.107 107% 3 12.80 0.005-5 0.9985 0.05 2.1 NF 0.095 95% 0.4 13.05 0.005-5 0.9990 0.05 0.9 NF 0.101 101% 0.01 13.15 0.005-5 0.9997 0.01 2.8 NF 0.097 97%
3
E-mail : [email protected]
2013 Thermo Fisher Scientific Inc.
A p
p lic
a tio
n N
o te
L C
M S
1 3
0 0
113.7%0.413.5%
3
%RSD
104.5 0.6 98.5 2.4 103.7 1.7 101.0 2.5 108.3 0.4 99.5 7.5 95.6 9.2 106.1 1.4 109.3 1.2 110.1 3.4 98.7 2.4 103.0 4.7 110.2 1.2 107.2 5.0 108.7 2.5 105.6 3.1 110.7 2.2 102.7 3.4 2,4-D 97.0 4.8 104.9 1.3 90.6 13.5 105.9 0.4 95.1 4.1 113.7 4.9 107.9 4.5 107.7 2.4 92.7 5.8 103.6 3.0 98.8 2.1
1/100
LC-MS29 10 mg/L 0.2% EDTA 10
mg/L 0.2% EDTA
A p
p lic
a tio
n N
o te
L C
M S
1 3
0 0
UltiMate™ 3000
Thermo Scientific
Acclaim™ RSLC 120 C18 2.2 µm 150 x 2.1 mm Part No: 071399
A 0.1% B 5%B0min→95%B10min→95%B14min
→5%B14.1min to 20min
0.2 mL/min
MS Thermo Scientific
Ar1.0 mTorr
1SRM Timed SRM
No Precursor m/z
Product m/z
CE eV
Start min
Stop min
1 + 231 156 12 5.51 7.01 2 + 163 88 10 6.55 8.05 3 + 279 264 20 7.88 9.38 4 + 295 217 20 8.09 9.59 5 + 190 163 24 8.85 10.35 6 + 224 41 13 9.39 10.89 7 + 241 88 14 9.58 11.08 8 + 222 165 14 9.82 11.32 9 + 295 280 19 9.86 11.36 10 + 355 88 14 10.01 11.51 11 + 311 125 40 10.03 11.53 12 - 239 132 28 10.09 11.59 13 + 202 145 12 10.10 11.60 14 + 408 182 22 10.78 12.28
15 + 411 149 22 10.85 12.35
16 + 233 72 20 10.86 12.36 17 + 404 372 15 10.91 12.41 18 + 263 231 25 10.98 12.48 19 2,4-D - 219 161 15 11.08 12.58 20 + 233 137 20 11.29 12.79 21 - 254 196 13 11.51 13.01 22 + 269 151 14 11.54 13.04 23 - 213 141 18 11.66 13.16 24 - 435 330 16 11.85 13.35 25 + 398 314 12 11.90 13.40 26 + 435 182 22 11.97 13.47 27 + 330 245 16 12.05 13.55 28 + 334 139 22 12.29 13.79 29 + 279 169 20 12.40 13.90
2SRM 1
20 % 1/100 1 /1000 .005 µg/L CV%=8.3%1/1000.01 µg/L 0.01 µg/L 5.4%
2
1/100 µg/L
RT min
µg/L R2
%
2 6.25 0.005-5 0.9998 0.05 1.6 NF 0.106 106% 0.3 7.31 0.005-5 0.9978 0.05 1.2 NF 0.097 97% 0.01 8.63 0.005-5 0.9996 0.01 3.0 NF 0.099 99% 0.01 8.86 0.005-5 0.9996 0.01 1.9 0.099 99% 0.8 9.61 0.005-5 0.9986 0.05 1.1 NF 0.101 101% 0.5 10.15 0.005-5 0.9994 0.05 4.6 NF 0.092 92% 0.2 10.33 0.005-5 0.9946 0.05 3.7 NF 0.086 86% 0.05 10.58 0.005-5 0.9982 0.05 1.1 NF 0.105 105% 0.01 10.62 0.005-5 0.9987 0.01 5.4 NF 0.105 105% 0.8 10.79 0.005-5 0.9993 0.05 3.8 NF 0.100 100% 0.01 10.79 0.005-5 0.9991 0.01 3.3 NF 0.100 100% 2 10.78 0.005-1 0.9954 0.05 1.8 0.098 98% 0.5 10.85 0.005-5 0.9969 0.05 1.5 NF 0.104 104% 0.3 11.53 0.005-5 0.9989 0.05 2.7 NF 0.097 97% 4 11.60 0.005-1 0.9978 0.05 2.1 NF 0.100 100% 0.3 11.61 0.005-1 0.9961 0.05 2.1 NF 0.098 98% 5 11.68 0.005-5 0.9966 0.05 4.3 NF 0.102 102% 0.01 11.74 0.005-5 0.9993 0.01 2.7 NF 0.099 99% 2,4-D 0.3 11.76 0.005-5 0.9994 0.05 3.9 NF 0.091 91% 3 12.05 0.005-5 0.9995 0.05 1.8 NF 0.100 100% 0.06 12.20 0.01-5 0.9975 0.05 8.8 NF 0.088 88% 8 12.29 0.005-5 0.9990 0.05 1.0 NF 0.103 103% 0.05 12.37 0.005-5 0.9992 0.05 1.8 NF 0.094 94% 0.005 12.61 0.005-1 0.9991 0.005 8.3 NF 0.098 98% 1 12.65 0.005-5 0.9974 0.05 2.5 NF 0.099 99% 3 12.71 0.005-5 0.9986 0.05 1.3 NF 0.107 107% 3 12.80 0.005-5 0.9985 0.05 2.1 NF 0.095 95% 0.4 13.05 0.005-5 0.9990 0.05 0.9 NF 0.101 101% 0.01 13.15 0.005-5 0.9997 0.01 2.8 NF 0.097 97%
3
E-mail : [email protected]
2013 Thermo Fisher Scientific Inc.
A p
p lic
a tio
n N
o te
L C
M S
1 3
0 0
113.7%0.413.5%
3
%RSD
104.5 0.6 98.5 2.4 103.7 1.7 101.0 2.5 108.3 0.4 99.5 7.5 95.6 9.2 106.1 1.4 109.3 1.2 110.1 3.4 98.7 2.4 103.0 4.7 110.2 1.2 107.2 5.0 108.7 2.5 105.6 3.1 110.7 2.2 102.7 3.4 2,4-D 97.0 4.8 104.9 1.3 90.6 13.5 105.9 0.4 95.1 4.1 113.7 4.9 107.9 4.5 107.7 2.4 92.7 5.8 103.6 3.0 98.8 2.1
1/100