タイトル

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. SM0ストマイ構造 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

9. SM0ストマイ2020 Streptomycin ( Shimadzu LCMS-2020 ) Mass chromatograms Dihydrostreptomycin 20 ng Streptomycin 20 ng Dihydrostreptomycin 20 ng Streptomycin 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

10. SM0ネオマイ8030chrm Neomycin (Shimadzu LCMS-8030) Mass chromatograms 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(+) Neomycin

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

12. LCMS-テトラサイクリン

13. SM0農薬8030 AgliChem (shimadzu LCMS-8030) 1:Glufosinate 182.00>136.00(+) MRM Chromatograms 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(+, -) 2:Diquat dibromide 184.05>158.05(+) 3:Acephate 184.00>143.00(+) 4:Fosetyl 109.00>81.05(-) 5:Dalapon 140.90>97.10(-)

14. LCMS-Wvit

15. SM0Wvit8030chrm 1: Thiamin 2400000 1:265.10>122.10 2:170.10>152.20 2300000 3:124.20>80.0 4:123.10>80.0 2: Pyridoxin 2200000 5:220.10>90.00 6:678.55>146.80 2100000 7:377.20>242.80 2000000 8:245.10>227.10 9:440.20>295.10 1900000 3: Nicotinic acid 1800000 1700000 4: Nicotinamide 1600000 1500000 5: Pantothenic acid 1400000 1300000 1200000 6: Cyanocobalamin 1100000 1000000 900000 7: Riboflavin 800000 700000 8: Biotin 600000 500000 9: Folic acid 400000 300000 200000 100000 0 -100000 0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 min W. Vitamin (Shimadzu LCMS-8030) MRM Chromatograms 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(+)

16. SM0Wvit8030Calib W. Vitamin (Shimadzu LCMS-8030) Calibration curves 1: Thiamin 2: Pyridoxin 3: Nicotinic acid 4: Nicotinamide 5: Pantothenic acid 6: Cyanocobalamin 7: Riboflavin 8: Biotin 9: Folic acid

17. SM0Wvit8030MRM 250000 1:265.10>122.10(+) 2:170.10>152.00(+) 3:124.00>80.00(+) 175000 225000 225 150000 200000 175000 125000 200 150000 100000 125000 175 75000 100000 150 75000 50000 50000 25000 125 25000 0 0 100 1.50 1.75 2.00 2.25 2.50 2.75 min 2.50 2.75 3.00 3.25 3.50 3.75 min 3.50 3.75 4.00 4.25 4.50 4.75 min 4:123.10>80.00(+) 5:220.10>90.00(+) 6:678.55>146.80(+) 450000 125 80000 400000 70000 100 350000 60000 300000 75 50000 250000 40000 200000 50 30000 150000 20000 100000 25 10000 50000 0 0 0 4.00 4.25 4.50 4.75 5.00 5.25 5.50 min 6.0 6.5 7.0 7.5 min 5.0 5.5 6.0 6.5 min 7:377.20>242.80(+) 8:245.10>227.10(+) 9:442.20>295.10(+) 25000 1500 3500 22500 3000 20000 1250 17500 2500 15000 1000 2000 12500 750 1500 10000 7500 1000 500 5000 500 2500 250 0 0 7.00 7.25 7.50 7.75 8.00 8.25 min 7.50 7.75 8.00 8.25 8.50 8.75 min 6.5 7.0 7.5 8.0 min W. Vitamin (Shimadzu LCMS-8030) Sample Preparation MRM Chromatograms 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: Thiamin 2: Pyridoxin 3: Nicotinic acid 4: Nicotinamide 5: Pantothenic acid 6: Cyanocobalamin *1:water/acetonitorile/acetic acid=94/5/1 *2:2 times for mix & heat 7: Riboflavin 8: Biotin 9: Folic acid

18. LCMS-WvitUSDA

19. LCMS-ViDOH

20. LCMS-PhosLipid

21. SM0H2Blocker H2Blocker (Shimadzu LCMS-2020) Mass chromatograms Mass spectra Cimetidine Ranitidine Cimetidine Famotidine 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

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