1. タイトル IMTAKT HPLC SEMINAR LC-MS Applications

2. ProdLine

3. 島津 LCMS2010A

4. LCMS-OctPhenol

5. LCMS- メタミドホス

6. LCMS- ジクロルボス

7. LCMS- メラミン

8. Streptomycin アミノグリコシド系抗生物質 ODS 表面での保持が期待できない 吸光団をもたない アミノ基を有する → イオンペアクロマトグラフィー / 質量分析が利用されてきた SM0 ストマイ構造

9. Streptomycin ( Shimadzu LCMS-2020 ) Mass chromatograms Streptomycin 20 ng Streptomycin 20 ng Dihydrostreptomycin 20 ng Dihydrostreptomycin 20 ng Imtakt Scherzo SM-C18 (2.0 mmI.D. x 150 mmL., 3 µm) 20 mmol/L ammonium acetate /20 mmol/L acetic acid, gradient ODS (2.0 mmI.D. x 150 mmL., 3 µm) 5 mmol/L heptafluorobutyric acid /acetonitrile = 85/15 SM0 ストマイ 2020

10. Neomycin Neomycin (Shimadzu LCMS-8030) Q3 scan Sample: 1 mg/mL LC Column: Imtakt Scherzo SM-C18 (2.0 mmI.D. x 150 mmL., 3 µm) Mobile phase A: 20 mmol/L ammonium acetate - water Mobile phase B: 20 mmol/L acetic acid - water Gradient program: 10%B(0 min)-90%B(14.0 min)-10%B(14.01-24 min) Flow rate: 0.2 mL/min Injection volume: 2 µL Column temperature: 40 ºC MS MS : SHIMADZU LCMS-8030 Nebulizing gas flow: 1.5 L/min Drying gas flow: 10 L/min DL temperature: 250 ºC BH temperature: 400 ºC Ionization: ESI(+) Mass chromatograms SM0 ネオマイ 8030chrm

11. [M+H] + [M+2H] 2+ Q3 Scan Product ion scan Precursor ion: m/z 615.3 Mass spectra 455 161 293 SM0 ネオマイ 8030mass Neomycin (Shimadzu LCMS-8030)

12. LCMS- テトラサイクリン

13. Sample: 1 µg/mL LC Column: Imtakt Scherzo SM-C18 (2.0 mmI.D. x 150 mmL., 3 µm) Mobile phase A: 5mmol/L ammonium formate - water Mobile phase B: 200mmol/L ammonium formate + 0.1% formic acid - acetonitrile Gradient program: 0%B(0 min)-100%B(10.0 min)-0%B(10.01-15 min) Flow rate: 0.2 mL/min Injection volume: 2 µL Column temperature: 40 ºC MS MS: SHIMADZU LCMS-8030 Nebulizing gas flow: 1.5 L/min Drying gas flow: 10 L/min DL temperature: 250 ºC BH temperature: 400 ºC Ionization: ESI(+, -) 5:Dalapon 140.90>97.10(-) 4:Fosetyl 109.00>81.05(-) 3:Acephate 184.00>143.00(+) 2:Diquat dibromide 184.05>158.05(+) 1:Glufosinate 182.00>136.00(+) AgliChem (shimadzu LCMS-8030) MRM Chromatograms SM0 農薬 8030

14. LCMS-Wvit

15. W. Vitamin (Shimadzu LCMS-8030) 0.01.02.03.04.05.06.07.08.09.0min -100000 0 100000 200000 300000 400000 500000 600000 700000 800000 900000 1000000 1100000 1200000 1300000 1400000 1500000 1600000 1700000 1800000 1900000 2000000 2100000 2200000 2300000 2400000 8:245.10>227.10 7:377.20>242.80 6:678.55>146.80 5:220.10>90.00 4:123.10>80.0 3:124.20>80.0 2:170.10>152.20 1:265.10>122.10 9:440.20>295.10 1: Thiamin 2: Pyridoxin 3: Nicotinic acid 4: Nicotinamide 5: Pantothenic acid 6: Cyanocobalamin 7: Riboflavin 8: Biotin 9: Folic acid Sample: 10 µg/mL LC Column: Imtakt Scherzo SM-C18 (2.0 mmI.D. x 150 mmL., 3 µm) Mobile phase A: 5mmol/L ammonium formate + 0.1% formic acid - water Mobile phase B: acetonitrile Gradient program: 0%B(0 min)-50%B(10.0 min)-0%B(10.01-20 min) Flow rate: 0.2 mL/min Injection volume: 1 µL Column temperature: 40 ºC MS MS : SHIMADZU LCMS-8030 Nebulizing gas flow: 1.5 L/min Drying gas flow: 10 L/min DL temperature: 250 ºC BH temperature: 400 ºC Ionization: ESI(+) MRM Chromatograms SM0Wvit8030chrm

16. 2: Pyridoxin3: Nicotinic acid4: Nicotinamide5: Pantothenic acid 6: Cyanocobalamin 7: Riboflavin9: Folic acid 1: Thiamin 8: Biotin Calibration curves SM0Wvit8030Calib W. Vitamin (Shimadzu LCMS-8030)

17. 7.507.758.008.258.508.75min 250 500 750 1000 1250 1500 9:442.20>295.10(+) 6.06.57.07.5min 0 25 50 75 100 125 6:678.55>146.80(+) 5.05.56.06.5min 0 10000 20000 30000 40000 50000 60000 70000 80000 5:220.10>90.00(+) 3.503.754.004.254.504.75min 100 125 150 175 200 225 3:124.00>80.00(+) 2: Pyridoxin3: Nicotinic acid 4: Nicotinamide5: Pantothenic acid6: Cyanocobalamin 7: Riboflavin 9: Folic acid 1: Thiamin 8: Biotin 10 tablets ↓ Add 10 mL diluting Solution* 1 and mix for 30 seconds then heat (65 ºC, 5 min) * 2 ↓ Mix for 30 seconds, Centrifuge(12,000 rpm, 5 min) ↓ Centrifuge of supernatant (3,000 rpm, 10 minutes) ↓ Filtrate (0.45 µm filter) of supernatant * 1 :water/acetonitorile/acetic acid=94/5/1 * 2 :2 times for mix & heat Sample PreparationMRM Chromatograms SM0Wvit8030MRM W. Vitamin (Shimadzu LCMS-8030)

18. LCMS-WvitUSDA

19. LCMS-ViDOH

20. LCMS-PhosLipid

21. H 2 Blocker (Shimadzu LCMS-2020) Cimetidine Ranitidine Famotidine Cimetidine Ranitidine Famotidine Imtakt Scherzo SM-C18, (2.0 mmI.D. x 150 mmL., 3 µm) 40 mmol/L ammonium acetate/acetonitrile = 80/20 0.3 mL/min, 40 ºC 100 µg/mL, 1 µL Mass chromatogramsMass spectra SM0H2Blocker

22. LCMS- 抗うつ剤

23. LCMS- モルヒネ

24. LCMS- マリファナ代謝物

25. LCMS-Volicitin

26. LCMS- リン脂質

27. LCMS- セラミド

28. LCMS- ホルモン代謝物

29. LCMS- 単糖

30. LCMS- 砂糖

31. LCMS- 配糖体（ソラニン）

32. LCMS-Proteomics

33. LCMS-Metabolomics

34. おわりに