????????????? ?LC/MS?????????????????? - PowerPoint PPT Presentation

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

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Title: LC/MS Author: Last modified by – PowerPoint PPT presentation

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Title: ????????????? ?LC/MS??????????????????


1
??????????????
????????????? ????? ???? ????? ??? ????
2
????
? ????? ???? ??????? (??????????) ?
??????????????
3
??
?????????? ??????????????
???????????? ????????????
??????? ?????????????
4
????? ????
??

??????
???????????
C15H12N2O2 252.3 mp 296?
C12H12N2O3 232.2 mp 175-179?
?????? ???????
??
??????
??? ?2??????? ??? ?2???????
???
5
???????????
??? ( )
? ?
6
????????????
???()
???????????
????????? ()
???()
??????
????????? ()
50?????????????
7
?????????
??????? ? ???????
251.1
231.1
232.1
252.1
m/z
m/z
??????
9.7 min.
???????????
Negative
4.8 min.
8
???????Positive????????
C15H12N2O2 252.3
m/z
253.0
??????140V
? 274.9
? 182.0
? 225.0
254.0
? 182 ( 253 - 71 )
? 225 ( 253 - 28 )
?
?
? 275 ( 252 23 )
? Na??
9
????1
????(?????????????)
500ml 10ml/min PS2
2ml 50???????
N2 1ml
10
????2
LC/MS?????
HPLC
MS
Instrument

Agilent 1100
Instrument

Agilent 1100 LC/MSD
Column

ZORBAX XDB C-18
Ionization

Electrospray
N2
(50 psi)
2.1x150mm, 3.5µm
Neblizer

N2
(10 l/min.) 340?
Mobile phase

A B 70 30
Drying gas

A 2mM CH3COONH4
Polarity

Negative
B CH3CN
Fragmentor

120 V Vcap3500V
Flow rate

0.2 ml/min.
SIM(m/z) ?????? ???????????
Oven temp.

40?

???
251 (M - H)- 231 (M - H)-

Injection vol.

5 µl

???
252 (M - H)- 232 (M - H)-
????(MS)
????(LC)
11
???
?????????
??????
Area
Area
80000
120000
60000
80000
40000
40000
20000
MDL 2.2 ppt
MDL 2.4 ppt
0
0
0
20
40
0
20
40
Amountppb
Amountppb
5100 ppb ?????? ???? gt 0.99
12
????
???????60 ppt (ng/L) ???????? (n7)
?? ??? ??? ?? ??
?? ??? CV? ??? CV?
??????????? 87.1 2.1 77.9 5.0
?????? 83.7 2.7 86.5 3.6
13
??????????
1.?????? ?????? (PHT) ??????????? (PB)
?????????? (CBZ)
???
???
2.????????? ??? A ????? ??????? 9?? B ?????
??????? 12?? ?? C ???? ???? 6??
A
????
???
C
B
14
??A
a
?????????
b
c
? ?
???? (?) ?2? ?25?
???? (?/?) ?2? ?10?
???? ????? ???? ???
??? ??? ???
d
e
f
h
i
g
15
??
a
b
c
d
e
f
h
i
g
n.d??????
16
??B
???
?????????
a
?
? ? ?
???? (?) ?10? ?5? ?2?
???? (?/?) ?2? ?1? ?0.5?
???? ??????? ??????? ???????
??? ??? ??? ??
b
c
?
d
???
e
f
g
j
?
l
h
k
?????????
i
??
??? ????? 9???? 2??? 1 ??
17
??
???
a
?
b
c
?
d
???
e
f
g
j
?
l
k
h
i
??
n.d??????
18
??C
????
??
A
B
C
D
E
F
n.d??????
19
???
1.???????????????????????????????????????????
(????? 2.2?2.4?0.2 ppt) 2.?????????????ppt?????
????? ???????????????
?????????????????? 3.????????????????
20
(No Transcript)
21
??????????
??????????????
????????????(S/N? 3.3 ? 29) 20????????????????

22
???????
??????
??????????? (34ppb)
?????? (4.2ppb)
5000
?????????? (1.0ppb)
4000
3000
2000
23
??????
?? 195 km
???? 7,861 km2
???? 90??
????? ?6?
?? 2 100?/sec
???? 12?ha (?85?ha??35ha)
24
???
?????????????????????
????????? ???????????????
lt?2???????gt ??????? 739?? ???????????????????
? ? ??????????
lt?1???????gt PCB? 13?? ???????????? ?
????????????????
lt?2???????gt ?????????? 23?? ?????????????????
? ? ???????????
lt?1???????gt ??? ?? ???????? ?
??????1t?????????????
lt?3???????gt ??? ?? ???????? ?
??????100t?????????????
25
???
??????????????????????????????????
?????????? ???????????????? ??????????
lt?1???????gt 354?? ??? or ????????? ????????
PRTR????
lt?2???????gt 81?? ??? or ????????? ??????????
?????????????(MSDS)???
26
??????????
????(?????) ??????? ??????????
???????????? ? ?????????????? ?????????????
27
??
??? ?? ???? LogPow ?? ??? ??
??????????? 232.24 174 1g/L 1.47 ??????? ??????? ???2? ???2 ?????? ?????
?????? 252.27 295(??) 32mg/L 2.47 ??????? ??????? ???2? ???2 ??????
?????????? 236.27 189-193 2.25 ??????? ?? ??????
?????? 179.22 134 760mg/L 1.58 ??????? ??????? ???2? ???1-52 ???? ???
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