???????(LC-MS/MS)???

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???????(LC-MS/MS)?????????????

• ??????????
• ???
• 2012.5

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• ????(C23H25ClN2)?????????,??????????????????????,?
  ?????????????,???????????,?????????

3

• ????????????????
• ??????
• 2002?5??????????????????????????????
• 2005?8?,?????????????????,?????????,??????????????
  ????????????????????,???????????????????9?1???????
  ???????????????
• ????( GB/T19857-2005 )1µg/kg

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????

• 1. ????????-?????????
• 2. ??LC-MS/MS????????,?(1)??????????????????,(2)??
  ?????????????????????,?(3)????????(MRM)???????????
  ?

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??(HPLC)???(MS)???

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

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

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(No Transcript)
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??????(ESI)?????
????
?????
Rayleigh Limit Reached
?????

???? (Coulomb Explosions)
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????????(ESI)??
?????/?????
?????
??
??
?????
???
???
???
???


Neutral Molecules Analyte Ions Clusters Salts
















?? N2
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ESI????
?????
?????
10
?????

• ??????????????????????,????????,??????(M/Z)??,??
  ??M/Z???????,?????

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• ????????????????(UVcos?t),???????????-(UVcos?t)
  ??????????,???????????????????????????

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?????????????

• ???????(MS/MS)????(QqQ)
• ???????????????????????
• MS1 CID MS2
• Q1 q2
  Q3

• ????????????????(MS1),???????,??????????????????(c
  ollisioninduced dissociation,CID),???????????,???
  ??,???????(MS2)????

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?????QQQ

• ???(Full Scan)
• ?????(Product ion Scan)
• ?????(MRM)

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(1) ???

• ?????????????????,?????m/z????????????????????????
  ???
• ??????????????????????????????????????????????????
  ?????? ?

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(2) ????? (product ion scan)
MS1 CollisionCell MS2

• ??Q1???SIM??,??????????m/z?????
• Q2????????????(CID)
• Q3?????,??Q2????????m/z????
• ?MS2??????????????????,??????????????????????

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• ???????????????????????????????????????,????m/z???
  ???,???????

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(3) ??????

• ??????(MRM)????????????
• ?????????????????
• ????A abc??Q1??A,Q2??A??a?b?c,
  Q3??a?b?c???,?????A abc?????????,???????A???
  ,?????A????

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MS1 CollisionCell MS2

• ???????????????,????????????
• ????Q1?Q2????,???????m/z????m/z????????????m/z????
  ?,????????????????,???????,??MRM???????

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LC-MS/MS(???,6410)?????
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• 1. ?????????????

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• 2. ????
• (1)????MassHunter ??????,??MassHunter???????
• ???????????????,???HPLC ?QQQ??????????

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• (2)?????????,?????,?????????????????????,?????????
  ??????
• (3)?????????????
• (4)????????????????
• (5)?MS QQQ ????, ?????????????,
  ????????Atune.TUNE.XML

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

• Time Segments ?????????????,???????????,????????,
  ????????????????????,???????????
• MS1 Res?MS2 Res??1???2????,??Unit?
• Fragmentor????,??????CID???????????fragmentor,???
  ?????????,????????????????????????????
• Collision Energy????,????CID?????????,???50V???
• Dwell????,????????????????

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• ???????????QQQ ??????Gas Temp., Gas Flow,
  Nebulizer, Capillary etc.

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3. ?????

• (1)????Agilent Masshunter Qualitative Analysis
  ??,???????
• (2)???????????,??Extract Ion Chromatogram,???Type
  ???,?m/z Values(s)?????????????,??OK ???

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• (3)????????,??Integrate(MS)????????
• ?????????????????????????

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????

• ??????LC-MS/MS?ESI????????????????????
• ????????,????H????????MH?????,????ESI????????

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???????

• ???????364.9

Ion Sourcex ESI
Ion polarity Positive
Gas Temp. 300?C
Gas Flow 11L/min
Nebulizer 35 psi
Capillary 4000 v
MS Res. Unit
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???????

• (1)?????,???????????m/z,??????????

Segment Name Start mass End mass Scan Time Fragmentor Polarity
MG 100 Positive
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???????

• (2)???????,???????????????????????????MRM???????,
  ???????????????????

Compound Precursor Ion MS2 from MS2 to Scan Time Fragmentor Collision Energy Polarity
MG 100 40 Positive
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???????

• (3)??????????????????,?MRM?????????,?????????????,
  ??2????????????

MRM??
Compound Precursor Ion Product Ion Dwell Fragmentor Collision Energy
MG 100 100 40
MG 100 100 40
??????(µg/L) 1 5 10 20 50
????
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????

• ???????????????
• ?????????????????????????????
• ?MRM??,????????????

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???

• ?????????

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5?21??????????????919,? ?