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1 LC/MS, LC/MS/MS 기초개론

2 LC LC/MS(Liquid Chromatography/Mass Spectrometry) 액상의분석물질을기화및이온화하여고진공관에서원하는질량 (m/z) 이나질량범위만검출하여정량 정성분석하는시스템 High vacuum PC/Software Ion source Mass Analyzer Detector ESI APCI APPI Quadrupole TOF Ion Trap EM PM Intensity [M+H] [M-A] + + A [M-B] + B

3 LC LC/MS(Liquid Chromatography/Mass Spectrometry) 액상의분석물질을기화및이온화하여고진공관에서원하는질량 (m/z) 이나질량범위만검출하여정량 정성분석하는시스템 High vacuum PC/Software Ion source Mass Analyzer Detector ESI APCI APPI Quadrupole TOF Ion Trap EM PM Intensity [M+H] [M-A] + + A [M-B] + B

Multimode Source ESI and APCI combined in one source Simultaneous operation

4 LC/MS Ion Sources Widest choice of sources from any manufacturer Dual electrospray (ESI) Dual nanospray APCI APPI CE-TOF PDF-MALDI Interchangeable between MS platforms Multimode Source ESI and APCI combined in one source Simultaneous operation HPLC-Chip/MS Nanospray made ease Reproducible results Sample processing on chip 대기압상에서분석물질이기화되고이온화되게하는장치

5 GC EI vs LC (ESI, APCI, APPI) GC/MS

6 LC/MS Ion Source-Application range

7 Ion Source 전기분무이온화 (ESI) 대기압력화학이온화 (APCI) 멀티모드소스 (MMI) + = 이밖에 APPI, HPLC Chip, PDF-MALDI 등 Page 7

8 Electrospray Ionization Sulfamethazin 279.1[M+H] + 301[M+Na] +

9 Atmospheric Pressure Chemical Ionization

10 LC LC/MS(Liquid Chromatography/Mass Spectrometry) 액상의분석물질을기화및이온화하여고진공관에서원하는질량 (m/z) 이나질량범위만검출하여정량 정성분석하는시스템 High vacuum PC/Software Ion source Mass Analyzer Detector ESI APCI APPI Quadrupole TOF Ion Trap EM PM Intensity [M+H] [M-A] + + A [M-B] + B

11 Single Quadrupole Mass Analyzer

12 Quardupole LC/MS 4개의평행한막대로구성되었고, 이온들이막대의중앙을통과하는과정에서막대에 RF/ DC 의비를일정하게유지하면서 DC 전위를변화시켜질량스펙트럼을얻게된다. + DC+RF + 경로차에의한질량분리 m/z time Abundance + + m/z

13 LC LC/MS(Liquid Chromatography/Mass Spectrometry) 액상의분석물질을기화및이온화하여고진공관에서원하는질량 (m/z) 이나질량범위만검출하여정량 정성분석하는시스템 High vacuum PC/Software Ion source Mass Analyzer Detector ESI APCI APPI Quadrupole TOF Ion Trap EM PM Intensity [M+H] [M-A] + + A [M-B] + B

14 Ion Detector 검출기에도달하는이온을전자로변환하여신호를증폭 Electron Multiplier Photo- Multiplier

미지물질의확인, peak purity, multiple charge를가지는물질의분자량결정에사용

15 Single Quadrupole scan mode Full scan 사용자가 mass range 를지정하여 monitoring 하는방식 순차적으로특정이온을 monitoring Scan mode는정성분석, 미지물질의확인, peak purity, multiple charge를가지는물질의분자량결정에사용 SIM(Selected Ion monitoring) 사용자가지정한이온만 monitoring 고감도및고재현성을가짐 정량분석이나기지의물질확인에이용

17 LC/MS/MS LC/MS 의첫번째질량필터로부터들어오는이온과비활성기체를충돌시켜조각난이온들을검출하여정량 정성분석하는시스템 Ion Optic Collision cell Capillary Lenses Q1 Q2 Q3 Page 17

18 LC MS, MSMS 정보는? Abundance HPLC RT 정성 1 차 Sulfamethazin 279.1[M+H] + 301[M+Na] + time + M/Z 1) 분자량확인 MS 2) 구조정보확인 MS/MS MS, MSMS 스펙트럼 정성 2 차 /3 차 Page 18

19 Triple Quadrupole Full Scan MS/MS parent ions enter collision cell - collide with argon gas and dissociate Detector API Source +/- ions and neutrals formed in API source ion guide transports +/- ions to Q1 Q1 is parked allowing only parent ions of a single m/z to pass to the collision cell Q3 is scanned passing full scan product ion spectra to the detector

20 Multiple reaction monitoring(mrm-cont.) High throughput_ Minimal sample preparation Both Qualitative and Quantitative information Multiple MRM Sensitivity transitions or full scan MS/MS spectra

21 QQQ Data Acquisition mode Q1 Collision cell Q3 MS scan MS SIM Product ion Precursor ion Neutral loss/gain MRM

22 QQQ MULTIPLE REACTION MONITORING (MRM) Page 22 Fragmentor Collision collision cell

1. Mass Spectroscopy 의기본원리 원자및분자를기체상 (high-vacuum region) 에서이온화시켜하전입자 ( 분자또는원자 ) 에대한질량 (mass/charge) 을측정하여 molecular weight을결정하는방법, 더나아가복잡한구조를가진화합물의구조

1. Mass Spectroscopy 의기본원리 원자및분자를기체상 (high-vacuum region) 에서이온화시켜하전입자 ( 분자또는원자 ) 에대한질량 (mass/charge) 을측정하여 molecular weight을결정하는방법, 더나아가복잡한구조를가진화합물의구조 의약외품 화장품품질확보를위한워크숍 GC/MS 및 LC/MS 의이해및응용 Matrix-Assisted Laser Desorption Ionization Timeof-Flight (MALDI- TOF) Electrospray Ionizationquadrupole-Timeof-Flight tandem MS (ESI-q-TOF tandem MS) Liquid Chromatography-