New Development in Sample Preparation

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? ? ? ? ? ? ? ?
New Development in Sample Preparation
Pretreatment Techniques
2
Preface
? ?
???????????????????????????????????????,??????
???????????????
3
Preface
????
????????????????? ???????(?????) ????????? ????
????(???) ????? ??????
4
????(sample preparation)??
Preface
?????????????????, ????????????????? ??????????(?
?)
???(pretreatment sampling)??
????????????????? ????????????????? ???,?????????
(??)
5
??????(??)
Preface
???? ?? ????
?????? (AutoSox) ?????? (ASE) ????????
(MASE) ??????? (SFE)
?? ?? ? ??
???? (SPE) ????? (SPME)
???? ???? ????
?????? (SLME) ??????? (MMLLE) ????? (LPME) ???
(EE) ???? (CCD)
??? (ME)
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Preparation
?????? sample preparation
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AutoSox
?????? Automatic Soxhlet Extraction
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AutoSox
????????????????????????
AutoSox???????????(???)?????(2-4hr??????))?
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AutoSox
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AutoSox
Gerhardt - SOXTHERM 2000
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ASE
?????? Accelerated Solvent Extraction
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??????????,????,??????????? ???????????
??????
?????????????? ???????(??????)
??????(??????) ????????????
ASE
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ASE
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ASE???SFE??,TltTc,PltPc,????SFE???,???SFE??,
??????????????
ASE
???????? ?????(15min)
????????????? ??????,????
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ASE
Dionex ??? ASE 100?300 ???
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MASE
???????? Microwave-Assisted Solvent Extraction
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MASE
???????????????????????,MASE??????????????
??MASE?,????????????(?????????)?,?????,?????
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MASE
MASE
OTHER
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???????
(1) ???????(?????) ?????????,??????????,??
?????????(??ASE?????) (2) ????????(?????)
???????,????????????????????????????????????????
????,??????????????????
MASE
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MASE???
MASE
(1) ????? (2) ??????????????????????,????????????
(3) ?????(10min)??? (4) ?????????(?ASE?SFE?????
???)?
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MASE
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MASE
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SFE
??????? Supercritical Fluid Extraction
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???????
SFE
? ???,???????? ? ???? ? ?????? ? ??????
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??????????
SFE
? ????,????? ? ????????? ? ??????? ?
????????
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??SFE???????
(1)???? (2)???? (3)??? (4)C02?? (5)??????? (6)????
????
SFE
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SFE???????????? ? ??????????? ?
???????? ? ?????????
SFE
?????????? ? ????(??????) ?
????(SPE)???????????????????????
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??????SFE??
? ????????? ? H2O?CHF3 ?CHClF3 ?N2O? SF6
???? ? ?????????????,???????
SFE
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Sampling
????? pretreatment sampling
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Sampling
EXAMPLE
Comparison of Naproxen spiked serum before(A)
and after(B) extraction using the C18 cartridge
and analysis by HPLC.
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?????????????? SPE?SPME
?????????????? SLME?MMLLE?LPME?EE?CCD
?????????????? ME
Sampling
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???? Solid Phase Extraction
SPE
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SPE???70??????,????????????????????????,???????
??
SPE
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SPE
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SPE
????
??????????
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1. Barbital 2. Allobarbital 3. Aprobarbital 4.
Phenobarbital 5. Butabarbital 6. Alphenal 7.
Hexobarbital 8. Amobarbital 9. Mephobarbital 10.
Secobarbital
SPE
Serum Extract Containing Barbiturates
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SPE??????
? ???SPE ? ???SPE ? ????? ? ????SPE
SPE
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???SPE
SPE???????????,??lt1mm,???496mm?
SPE
dSPE???cSPE?????????????,?????????,???????,???
????????????????,?????????????????
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SPE
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???SPE
??SPE???????A???????,??????B????????SPE????SPE
???????????,?????????? ???SPE????????????????,
???????????????
SPE
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SPE
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?????
???(Restricted Access,RA)??,??????????????
?????(Internal Surface Reversed Phase)
?????(Semi-permeable Surface)
??????(Shielded Hydrophobic Phase)
?????(Mixed Functional Phase)
SPE
???????(molecular imprinting
sorbents,MIPs),??????????
?????????????
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SPE
Schematic of the molecular imprinting principle,
in which the template is the structural analogue
of the target analyte.
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SPE
LC chromatogram obtained after preconcentration
of a 100 mL groundwater sample on (a) a
non-imprinted polymer and (b) terbuthylazine-impri
nted polymer.
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????SPE
?????????????,?????????????????,??????????????
???????,????????????????,???????????????,?????????
??
SPE
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SPE
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???? SPE ??
???? SPE ?? SPE ?? SPE fluorous SPE
SPE
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SPE
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Merrifield L.???????SPE??????????????????!
SPE
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????? Solid Phase Micro-extraction
SPME
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SPME????????????,?????????????????????????????
?????????????????????(???GC,?HPLC)?,??????????(??
????,?????),?????????
SPME
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SPME
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SPME
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??SPME??????????? ??? ??SPME???????,??
? ??SPME???????? ????????????
SPME
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SPME
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SPME
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SPME
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SPME
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SPME
Pesticides analysis by SPME/Ion Trap MS
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SPME???
? ????????? ? ???????????? ???,???????? ?
??????(????) ? ???????
SPME
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SPE?SPME?????
SPE SPME
SPME
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SPE SPME
SPME
?(micro)SPE?SPME