LC-MS Klinisk Kemi

Region Skåne

Anders Blomgren

Utbildningsdagar, Saltsjöbaden

8:e feb 2017

Innehåll

• Region Skåne, SUS, Klinisk Kemi

• LC-MS verksamheten

- Lokaler/Instrumentering/Arbetssätt

- Analyserna

Klinisk Kemi, Region Skåne

Universitetssjukhus

Närsjukhus

Akutsjukhus

Klinisk Kemi, Region Skåne

Klinisk Kemi, Region Skåne

• LC-MS system på Klin Kem före 2015

- 2 i Lund, 2 i Malmö och 1 i Helsingborg

• 2013 - Samlokalisering Masspektrometri- kritisk massa

- samlad kompetensen

- åldersavgångar

- bättre utnyttjande av instrumenten

Ombyggnation – befintligt och nytt MS-lab

Sista systemet flyttat jan 2016

Ombyggnation MS lab

• Media

• Högt ljud

• Värme/Kyla/Drag

• Serviceåtkomst

• Visuell kontakt

Nytt lab Ombyggt lab

Ombyggnation MS lab

• Enhetligt (mjukvara, instrument)

• Tidsplan för utbyte

Provupparbetning

Provupparbetning

Robotar

- är snabba

- ger bra precision

- gör likadant varje gång

- blir inte uttråkade

- är enkla att reparera

Metoder

- proteinfällning så länge det går

- fällningsplatta

- SPE (3 robotar utrustade)

- (2D-LC)

Personal

Kemister, 5 st

• Läkemedel

• Missbruk

• Endokrinologi

• Protein

• Robot (ny)

Benny Larsson

Therese Hansson

Per Bengtsson

Maria Fröjd

Anders Blomgren

Läkemedel

U/P-Metoxykatekolaminer

U-Kortisol

Analyserna

Utveckling

Utbildning

Steroider (Östradiol

Androstendion

Testosteron

17OH-Progesteron)B-PEth

S-Metformin

S-Vit D

S-MMA

S-Hepcidin

XIC of +MRM (22 pairs): 315.200/58.200 amu Expected RT: 3.0 ID: S-Klomi from Sample 8 (Antidep kont hög) of ADEPR_160629_78A.wi... Max. 4.8e6 cps.

0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0 3.2 3.4 3.6Time, min

0.0

2.0e5

4.0e5

6.0e5

8.0e5

1.0e6

1.2e6

1.4e6

1.6e6

1.8e6

2.0e6

2.2e6

2.4e6

2.6e6

2.8e6

3.0e6

3.2e6

3.4e6

3.6e6

3.8e6

4.0e6

4.2e6

4.4e6

4.6e6

4.8e6

Inte

ns

ity

, c

ps

2.99

Antidepressiva

XIC of +MRM (5 pairs): 975.400/908.500 Da ID: B-Evero from Sample 8 (immuno kont hög) of IMMUN_160705_37A.wiff (Turbo Spray) Max. 5.1e5 cps.

0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8Time, min

0.0

5.0e4

1.0e5

1.5e5

2.0e5

2.5e5

3.0e5

3.5e5

4.0e5

4.5e5

5.0e5

5.5e5

6.0e5

6.5e5

7.0e5

7.5e5

8.0e5

8.5e5

9.0e5

9.3e5

Inte

ns

ity

, c

ps

1.70

Immunosuppressiva

XIC of +MRM (10 pairs): 438.200/171.200 Da ID: Flufenazin from Sample 8 (LCMS1 kont hög) of LCMS1_160704_25A.wiff (Turbo Spray... Max. 3.7e6 cps.

0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 1.9 2.0 2.1 2.2 2.3Time, min

0.0

5.0e5

1.0e6

1.5e6

2.0e6

2.5e6

3.0e6

3.5e6

4.0e6

4.5e6

5.0e6

5.5e6

6.0e6

6.5e6

7.0e6

7.5e6

8.0e6

8.3e6

Inte

ns

ity

, c

ps

1.46

Neuroleptika 1

XIC of +MRM (16 pairs): 411.200/191.100 amu Expected RT: 1.6 ID: S-Rispe from Sample 8 (LCMS2 kon hög) of LCMS2_160704_29A.w... Max. 4.0e6 cps.

0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2Time, min

0.0

5.0e5

1.0e6

1.5e6

2.0e6

2.5e6

3.0e6

3.5e6

4.0e6

4.5e6

5.0e6

5.5e6

6.0e6

6.5e6

7.0e6

7.5e6

8.0e6

Inte

ns

ity

, c

ps

1.57

Neuroleptika 2

Biphenyl

BiphenylBiphenyl

Biphenyl

Antiarytmika Bensodiazipiner

Antiepileptika

XIC of +MRM (14 pairs): 645.800/58.000 amu Expected RT: 3.8 ID: Amiod-S from Sample 8 (LCMS4 Kon Hö) of LCMS4_160629_27A.wif... Max. 2.9e6 cps.

0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5Time, min

0.0

2.0e5

4.0e5

6.0e5

8.0e5

1.0e6

1.2e6

1.4e6

1.6e6

1.8e6

2.0e6

2.2e6

2.4e6

2.6e6

2.8e6

3.0e6

3.2e6

3.4e6

3.6e6

3.8e6

3.9e6

Inte

ns

ity

, c

ps

3.63

XIC of +MRM (22 pairs): 389.100/245.100 amu Expected RT: 0.9 ID: Zopik-S from Sample 8 (LCMS6 kon hö) of LCMS6_160630_02A.wi... Max. 2.4e6 cps.

0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0Time, min

0.0

5.0e5

1.0e6

1.5e6

2.0e6

2.5e6

3.0e6

3.5e6

4.0e6

4.5e6

5.0e6

5.3e6

Inte

ns

ity

, c

ps

1.00

XIC of +MRM (8 pairs): 219.190/162.100 amu Expected RT: 1.1 ID: Primidon from Sample 8 (LCMS7 kon hö) of LCMS7_160705_27A.wiff... Max. 3.0e6 cps.

0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0Time, min

0.0

2.0e5

4.0e5

6.0e5

8.0e5

1.0e6

1.2e6

1.4e6

1.6e6

1.8e6

2.0e6

2.2e6

2.4e6

2.6e6

2.8e6

3.0e6

3.1e6

Inte

ns

ity

, c

ps

1.08

B-PEth 16:0/18:1

XIC of -MRM (9 pairs): 701.400/255.200 Da ID: Peth 16:0 18:1_255 from Sample 10 (PEth kont Hög) of LCMS8_160706_68A.wiff (Turbo ... Max. 1.0e6 cps.

0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4Time, min

0.0

1.0e5

2.0e5

3.0e5

4.0e5

5.0e5

6.0e5

7.0e5

8.0e5

9.0e5

1.0e6

1.1e6

1.2e6

1.3e6

1.4e6

1.5e6

1.6e6

1.7e6

1.8e6

1.9e6

2.0e6

2.1e6

2.2e6

2.3e6

Inte

ns

ity

, c

ps

1.25

1.42

C18

Biphenyl

Biphenyl

Biphenyl

U-MetoxikatekolaminerEtG/EtS

Metformin MMA

XIC of +MRM (6 pairs): 166.075/134.200 Da ID: U-MNA from Sample 5 (METOX kon hö) of METOX_160704_13A.wiff (Turbo Spray) Max. 1.0e6 cps.

0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0 3.2 3.4 3.6 3.8 4.0 4.2 4.4 4.6 4.8Time, min

0.00

5.00e4

1.00e5

1.50e5

2.00e5

2.50e5

3.00e5

3.50e5

4.00e5

4.50e5

5.00e5

5.50e5

6.00e5

6.50e5

7.00e5

7.50e5

8.00e5

8.50e5

9.00e5

9.50e5

1.00e6

1.04e6In

te

ns

ity

, c

ps

2.08

XIC of -MRM (8 pairs): 125.000/97.000 Da ID: EtS quant from Sample 8 (Hk) of 160111_BlankU_sp_vatten.wiff (Turbo Spray) Max. 7.8e6 cps.

0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0Time, min

0.0

5.0e5

1.0e6

1.5e6

2.0e6

2.5e6

3.0e6

3.5e6

4.0e6

4.5e6

5.0e6

5.5e6

6.0e6

6.5e6

7.0e6

7.5e6

7.8e6

In

te

ns

ity

, c

ps

2.18

XIC of +MRM (12 pairs): 130.100/70.800 Da from Sample 8 (Metformin Kon Hög) of METFO_160414_20A.wiff (Turbo Spray) Max. 4.5e5 cps.

0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5Time, min

0.0

2.0e4

4.0e4

6.0e4

8.0e4

1.0e5

1.2e5

1.4e5

1.6e5

1.8e5

2.0e5

2.2e5

2.4e5

2.6e5

2.8e5

3.0e5

3.2e5

3.4e5

3.6e5

3.8e5

4.0e5

4.2e5

4.4e5

In

te

ns

ity

, c

ps

2.69

XIC of -MRM (2 pairs): 116.800/72.800 Da ID: MMA from Sample 6 (MMA kon hög) of MMA_160705_52A.wiff (Turbo Spray IonDrive) Max. 2.3e5 cps.

0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 0.90 0.95 1.00 1.05 1.10 1.15Time, min

0.0

2.0e4

4.0e4

6.0e4

8.0e4

1.0e5

1.2e5

1.4e5

1.6e5

1.8e5

2.0e5

2.2e5

2.4e5

2.6e5

2.8e5

3.0e5

3.1e5

In

te

ns

ity

, c

ps

0.38

0.78

Lång C18

HILICZIC-HILIC

Hydrofil C18

XIC of +MRM (6 pairs): 166.075/134.200 Da ID: P-MNA from Sample 1 (Sample001) of Kal 3 10 ul 161130SET1.wiff (Turbo Spray) Max. 2.0e4 cps.

0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5Time, min

0.0

2.0e4

4.0e4

6.0e4

8.0e4

1.0e5

1.2e5

1.4e5

1.6e5

1.8e5

2.0e5

2.2e5

2.4e5

2.6e5

2.8e5

3.0e5

3.2e5

In

te

ns

ity

, c

ps

4.43

P-Metoxikatekolaminer

HILIC

XIC of +MRM (2 pairs): 558.800/693.800 Da ID: Hep 559/694 from Sample 9 (HEPCI kon hög) of HEPC_160706_36A.wiff (Turbo Spray I... Max. 1.7e4 cps.

0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8Time, min

0.0

1000.0

2000.0

3000.0

4000.0

5000.0

6000.0

7000.0

8000.0

9000.0

1.0e4

1.1e4

1.2e4

1.3e4

1.4e4

1.5e4

1.6e4

1.7e4

In

te

ns

ity

, c

ps

0.98

Hepcidin

C18

XIC of +MRM (12 pairs): 331.200/97.000 Da ID: 17OHP 1 from Sample 7 (kal 5) of Steroid 121212SET1.wiff (Heated Nebulizer) Max. 2.4e4 cps.

0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5Time, min

0.0

1000.0

2000.0

3000.0

4000.0

5000.0

6000.0

7000.0

8000.0

9000.0

1.0e4

1.1e4

1.2e4

1.3e4

1.4e4

1.5e4

1.6e4

1.7e4

1.8e4

1.9e4

2.0e4

2.1e4

2.2e4

2.3e4

2.4e4

In

te

ns

ity

, c

ps

3.97

U-kortisol S-Testosteron*

S-Vitamin D S-Androstendion

XIC of +MRM (4 pairs): 383.313/211.200 Da ID: VitD3 1 from Sample 4 (VITD L2) of VITD_160706_69A.wiff (Heated Nebulizer) Max. 3.2e4 cps.

0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6Time, min

0.0

5000.0

1.0e4

1.5e4

2.0e4

2.5e4

3.0e4

3.5e4

4.0e4

4.5e4

5.0e4

5.5e4

6.0e4

6.5e4

6.8e4

In

te

ns

ity

, c

ps

1.39

1.49

XIC of +MRM (11 pairs): 287.200/97.000 Da ID: Androstenedione 1 from Sample 10 (ANDRO Kon Hö) of ANDR_160628_43A.wiff (Heate... Max. 2.2e5 cps.

0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5Time, min

0.0

1.0e4

2.0e4

3.0e4

4.0e4

5.0e4

6.0e4

7.0e4

8.0e4

9.0e4

1.0e5

1.1e5

1.2e5

1.3e5

1.4e5

1.5e5

1.6e5

1.7e5

1.8e5

1.9e5

2.0e5

2.1e5

2.2e5

In

te

ns

ity

, c

ps

4.01

3.40

3.80

XIC of -MRM (6 pairs): 270.992/143.128 Da ID: Östradiol 1 from Sample 7 (ESTRA Kon Hö) of ESTRA_160630_26A.wiff (Turbo Spray) Max. 2176.0 cps.

0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 11.0 11.5 12.0 12.5Time, min

0.0

1000.0

2000.0

3000.0

4000.0

5000.0

6000.0

7000.0

8000.0

9000.0

1.0e4

1.1e4

1.2e4

1.3e4

1.4e4

1.5e4

1.6e4

1.7e4

In

te

ns

ity

, c

ps

5.91

S-Östradiol

XIC of -MRM (4 pairs): 407.100/331.200 Da ID: Kortisol 331 from Sample 8 (U-kort hög) of STER1_160630_04A.wiff (Turbo Spray) Max. 8.5e5 cps.

0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0Time, min

0.0

5.0e4

1.0e5

1.5e5

2.0e5

2.5e5

3.0e5

3.5e5

4.0e5

4.5e5

5.0e5

5.5e5

6.0e5

6.5e5

7.0e5

7.5e5

8.0e5

8.5e5In

te

ns

ity

, c

ps

1.62

XIC of +MRM (3 pairs): 292.200/96.800 Da ID: Testosterone d3 from Sample 4 (kal 4) of Testo körning 150121SET1.wiff (Heated Nebuliz... Max. 1.1e5 cps.

0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5Time, min

0.00

5000.00

1.00e4

1.50e4

2.00e4

2.50e4

3.00e4

3.50e4

4.00e4

4.50e4

5.00e4

5.50e4

6.00e4

6.50e4

7.00e4

7.50e4

8.00e4

8.50e4

9.00e4

9.50e4

1.00e5

1.05e5

1.10e5

1.14e5

In

te

ns

ity

, c

ps

3.68

2.86

XIC of -MRM (7 pairs): 359.100/331.100 Da ID: Aldo 2 from Sample 7 (k6) of Aldosteron 141124SET1.wiff (Turbo Spray) Max. 1.4e4 cps.

0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0 3.2 3.4 3.6 3.8 4.0 4.2 4.4 4.6 4.8Time, min

0.0

2000.0

4000.0

6000.0

8000.0

1.0e4

1.2e4

1.4e4

1.6e4

1.8e4

2.0e4

2.2e4

2.4e4

2.6e4

2.8e4

3.0e4

In

te

ns

ity

, c

ps

2.34

S-Aldosteron* S-17-HO-Progesteron*

* Inte tagen i bruk än

Biphenyl

2D-LC, C82D-LC, C18C18

2D-LC 2D-LC2D-LC

Analyserna

Drugs of abuse

Verifiering

Drugs of abuse

Verifiering

(Kannabinoider)

S-Transferrin proteoformer

Apo1-Lipoprotein

1-antitrypsin

Fria lätta kedjor

Kannabinoider (THC-COOH)

XIC of -MRM (4 pairs): 343.200/299.100 Da ID: THC-COOH 1 from Sample 13 (971231-3056) of DROG1_170104_10A.wiff (Turbo Spray ... Max. 3.7e5 cps.

0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5Time, min

0.0

2.0e4

4.0e4

6.0e4

8.0e4

1.0e5

1.2e5

1.4e5

1.6e5

1.8e5

2.0e5

2.2e5

2.4e5

2.6e5

2.8e5

3.0e5

3.2e5

3.4e5

3.6e5

Inte

ns

ity

, c

ps

2.81

S-Transferrin proteoformer

…+41 +40 +39 +38 +37…

-1-antitrypsin

Biphenyl

(2D-LC, affinitet & C4)

(2D-LC, affinitet & C4)

Fria lätta kedjor (2D-LC, affinitet & C4)

Problem / Hot

• Personalo Åldersavgångar

o Antal

• ITo Föråldrat

o Remisser

o Resurser

Tack!