Title: (Mass Spectrometry, MS)
1???? ??? (Mass Spectrometry, MS) ???
??????????(Mass Spectrograph) ????????
????????? ?????? ??? ???????
????? (Mass Spectrum) ???????
???????? ???????? ??? ??????(Hyphenated
method)
2?? ??????????????,???????????? a) ???
??? b) ?????????????---????,?????????(??
???) c) ????????????------???????(GC-MS) d) ???
????????-----????????---???? ???????????
3?? 1813?Thomson??MS???Ne??22Ne?24N????????
?,?????????? ?30????????????,???????????????
????????????,????????????????
?????????????? 40??????MS???????????,?????????
?? 50????????????,????????????????
???????NMR?IR??????????????????
??? 80??????????????????????MS??? 90???????????
,???????????????? ??????????GC-MS,HPLC-MS,G
C-MS-MS,ICP-MS ???????
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71. ???? ????,????????????????????(10-4-10-6??m
mHg?), ??????????????????,???? a)??????????? b)?
?????????,??????? c)????????? d)????????????????
??
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9b) ?????????????? ???????????25cm?6mm
i.d.,???????????(??),????????????????,?????
?? 1)??????,????? ???? 2)????????? 3)????
??
c) ??????????????????,??????,?????????????
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12EI
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15EI
FI
FD
16e) ???(Spark) ?????????????????????????,??
?AES??????? ? ?30kV ????---??---??????---????--
-?????---??????????? ? ?????????,???????(60???)?
??????????? f) ?????(Fast atom bombardment,
FAB) ? ????????????????????????????????
??????????????????
FAB
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18- ?????????,???(???B)???,??????(?????r)?????
Bev ???? mv2/r ???,?????????,?, - e?????U??????
- ?? (????),??????,
-
- ?B?r?U??????????????????????,??????
- ??B?U,??r,?????????????????r??????????????????m/z
??????(mass spectrograph) - ??????????r??,??????U???B,???m/z????????????????
???(Mass Spectrometer)?
19??????????????????????
???????????m/z ?????????????????(?
????????)? ???m/z ?????(???)?????????,?????
??,???5000?
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25??????????????????
26??? ??????? ????? ????m/z????,????(?????,
???????100)????(????,abundance)??????????,???????
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313)????? ????????????????????????,???????????
?????????????????? 4)????? ??????m1???????,??????
?????m???m2(??m1????,??????????)?????????m,??????
??m1?m2????,?????,??????????
???????????(?????m1????m2???)? 5) ????
??????????,?????????M1,M2??,???????????????????
32 ?????????? ????M1???m/z???,????????
???????,?????,??????!
33?? ???????m/z22.8???????,???????m/z86?m/z
44?????m/z101? m/z44???m/z86??????????????????????
??????? m22.8 ? 442/86 22.5
H
CH3
CH2
CH3
CH3
CH3-CH-NH-CH
m/z86
CH-NH-CH
CH3
CH3
CH3
m/z101
CH3-CHCH2(????)
CH3-CHNH2 m/z44(??)
34 ?????????????????,?????????????????????????
?????????? ?????????????????
35- ????????
- 1??????
- ????????????????,???????????????,
- ???????????????,??????????????????
- ??????,???????????
- ????????????????
- ???????????????????(?????)gt??gt?????gt????
gt????gt??gt?gt?gt?gt?gt?gt??gt???gt?gt??gt??gt?? - ??????
- 1)?????????,?????????????????,????
- ??????????(MH)??????????????(M-H)?
- 2)????????????C?H?O???????,????????
- ????????C?H?O?N????,????N???????,
- ????N????????????????????????
36- 3)????????????????????????????????????H?CH3?H2O?C
2H5.,?????????M-1,M-15,M-18,M-28??,??????M-3,M-1
4,M-24??,???????,???? ????????? - ????(4-13)?19-25?37?38?50-53?65-66??????
??,? - ???14CH2????,????????????????
- 4)??????????????????????????,??????????????3?????
??(M-CH3 ?? M-H2O?)? - ?????????????
- 1)????????????????(?????????,??????????????)?
- 2)?????????????????????
- 3)?????????,??????????????????????????????????????
????????????
37- 2???????
- ???????????????????????????CO?N2???
- ??m/z??28,??????????28.0040?27.9949,????????
- ????
- b) ??????????m/z?????????,?CO?N2????????
- ???????????????
- ?????CwHxNyOz,???????(M1)?(M2)???????????
??
38?1?????C8H12N3O?M1,M2????M????? ?? I(M1)
1.12?8 0.016 ?12 0.38 ?3 0.04 ?1
10.31 I(M2) 1.21 ?82/200 0.20 ?1
0.597 ??,I(M)I(M1)I(M2) 10010.310.597
39 ????Cl, Br, S ??????????????,?????????????(a
b)n?????,??a?b????????????????,n
????????????? CH3Cl??,a3, b1, n1,
??(31)131 ?m/z50(M)m/z52(M2)3
1 CH2Cl2??,a3, b1, n2, ??(31)2961,
?m/z84(M)m/z86(M2)m/z88(M4)961 C
HCl3??a3, b1, n3, ??,(31)3272791
?m/z118(M)m/z120(M2)m/z122(M4)m/z124(M
6)272791 ?????????????,??(a1b1)n1(a2b2)n2
??? ClCH2Br (31)1(11)1341 (35Cl,
37Cl 79Br, 81Br)
?m/z128(M)m/z130(M2)m/z132(M4)341
403????? a) ?????,????????????????????m/z??????????
,???????????,????????? b) ????????????.
41???????? ?????????????????????? 1??????????
???????????? a)C6D6?????C6D6,C6D5H,C6D4H2,C6D3
H3????? ???? b)?????????????????,?????????
???????????????????,????????
?????????????18O???,??????18O???
???????,???????????????????
??????? c)?????????36Ar?40Ar??????40Ar(?40K?1.3?
109 a ????)??,??????????? 2???????ICP-MS(?
???)
42?????
43??? ?????????(He???,??????????????)MS??? ??
?????????????? ???? ????????? ??????
?????????????????????????????????(Total ion
chromatogram, TIC) ???????(????)????,????MS?????
??????GC-MS???????????????(WHY?)?
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