Transcription of SIGMA-ALDRICH HPLC MS/MS A B - aisti.co.jp
1 - (1/1) .. 1 . (1) .. (2) .. ( ) Merck ( ) . SIGMA-ALDRICH (PURELAB Ultra ). Smart-SPE . 2 . 50mLPP 10g . 15 . 3 . ST-L300( ). HPLC Prominence( ). MS/MS API3200(AB Sciex). TSK gel SuperIC-AP( ). A . B . 100uL. 20min 40 . ESI Negative -4500V. 350 . MRM(Multiple Reaction Monitoring).. Time(min) 0 5 14 15 20. A(%) 5 50 50 5 5. B(%) 95 50 50 95 95. 4 . 10g 50mLPP - (1/1)30mL.. 10 (3500rpm 10min). 50mL . 4mL 1mL 1mL . ST-L300 .. HLBi3-20 SCX-30 PSA-50 2mL - (1/9) 2mL .. 1mL . - (1/9)1mL . HLB SCX PSA 1mL .. 1mL LC- MS/MS . 10 g - 1/1 30 mL. 10 min 10 min - 1/1 50mL . 1mL 1mL . 10 / . 1 mL. HLB. SCX-30. PSA-50 PSA-50 HLB SCX . - 1/9 1 mL NH3 1 mL.. 1mL . LC- MS/MS ..1 .. 1 LC . HPLC . ODS .. HPLC .. 1) . LC LC LC .. 2 ..2 (100ppb). 2 pH .. pH . pH pH . LC- MS/MS 3 .. LC-MS(/MS) .. pH 2 pH 7 pH 10..3 pH . 3 .. - (1/1) .. - (1/1) . 4 . (1) .. PSA . 4 .. O - O - HO O HO O. O P- O O P- O. O NH O P NH2 O NH O P NH2. - - - - O O O O. + +. H3N NH3 H2N NH2. +. NH2 PSA NH2. +. NH PSA NH. SiO SiO.
2 4 PSA ( ) ( ) . (2) . 1) 2) .. HLB SCX PSA . 1 5 .. HLB SCX PSA (106) (96). HLB SCX SAX (133) (22). HLB WAX PSA (51) (3). C18 SCX PSA (75) (4). 1 . 10 g - 1/1 30 mL. 10 min 10 min - 1/1 50mL . 1mL 1mL . 1 mL. HLB. SCX-30. PSA-50 PSA-50 HLB SCX . - 1/9 1 mL NH3 1 mL..5 . PSA SAX . PSA 2 NH NH2 . N+(CH3) 1 SAX .. 5 . ST-L300 RC(Remove and Connecting) .. HLB SCX PSA ..5 RC PSA . 6 .. SCX . PSA .. (n=5) RSD.. (%) (%). Glufosinate Glufosinate 3 .. LC .. pH .. - (1/1) PSA .. HLB SCX . ST-L300. RC .. 1) LC- MS/MS . (2013). 2) . Ann. Rep. Tokyo Metr. ,57,235-238,2006. 3) LC- MS/MS . 35 92-97. 4) LC/ICP/MS . 23 14, 10-14, (2011).
