LC/MS???????????? ?????????????????????????

1
LC/MS?????????????????????????????????????

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• ?????? ?? ??
• ???(?) ?? ??
• ??????????????(?) ?? ??

2
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• ????????????,
• LC/MS??????????????????????????

3
??????????
4
?????????????
?????? (GLYP)
???? (FOSE)
??????? (GLUF)
5
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??????????????? ?????????????????? ???????????????
?????????????? MCPA?????????, MDBA?????????, ????
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????????? ?????,DCMU, ????????, ??????????
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???A? ????EPAC ??????????? ?????????, ????,??
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???A? ????EPAC ?????????, ?????,??? ??????????
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???A? ????EPAC ?????????, ????,????
6
?????(???)

• HPLC?????
• FMOC-Cl????????????????????
• ??HPLC??????????????????????????

Glyphosate
FMOC-Cl
GLYP-FMOC
GC/MS????? MTBSTFA,TFAA-TFE??????????????????
Journal of Chromatography A, 907 (2001)
7
?????(????)
Prepare Sample pH 6-8
??????????????????PS2,C18?????????????????????????
?!
Condition 2mL methanol 4mL 0.5M NaOH, 2mL H2O
Rinse 4mL 0.5M NaOH Rinse 2mL H2O
Load 25mL sample
GLYP,GLUF,FOSE?????? ??????????!
Wash2mL H2O
Paraquat, Diquat???????
Elute 4mL 0.5M HCl in acetonitrile
Evaporate and Reconstitute adjust to pH 3 for
LC analysis
Waters OASIS Environmental Agrochemical
Applications Notebook
8
LC/MS????Paraquat, Diquat????
??????,??????????,????????????? ????????????(0.1µg
/L???????????!)
?12????????(2003)
9
??????
???????????????????????????LC/MS???,

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GLUF,GLYP,FOSE?????????????????????
??????,?????????????????????????
10
?????????
AMPA (m/z110)
GLUF (m/z180)
FOSE (m/z109)
Scan???,10mg/L,100µL???
11
?????????
SIM???,100µg/L,100µL???
12
????
13
??? 1, 10, 100µg/L100?L???
??????????????,??????? ????????????1
?g/L??????????
14
????????
?????????????,0.45?m???????????????? ?????????????
???????????
15
?????????(??7???????????)
?????1?g/L,?????0.1?g/L
16
???

• ?????????????????
• ESI????LC/MS????????????
• (AMPA????????????????)
• ????????????????,????????????????????????????????
  ???????????
• ????????
• ??????,?????,????????????GLYP,FOSE???????????????

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