Hydrocortisone Sodium Phosphate 3.5 1.0 0.5 1 μg/ml 3.0 2.5 25 ng/ml 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 min 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 min Fig.1 Chromatograms of Hydrocortisone Sodium Phosphate Instrument : Shimadzu NexeraXR+ LCMS2020 Column : Mastro TM C18(100 mml. 2.1 mmi.d., 3 µm) Typical C18(100 mml. 2.1 mmi.d., 3 µm) Flow Rate : 0.2 ml/min Detection : MS (SIM mode) Mobile Phase : A: 0.1% Formic Acid in Water B: 0.1% Formic Acid in MeCN 0.01 min ポンプ B.Conc 10% 5.00 min ポンプ B.Conc 80% 5.01 min ポンプ B.Conc 10% 6.50 min ポンプ B.Conc 10% Column Temp. : 40 Injection Vol. : 2 µl
Adenosine Triphosphate Adenosine Monophosphate 0.0 1.0 2.0 3.0 4.0 5.0 6.0 min 0.0 1.0 2.0 3.0 4.0 5.0 6.0 min Fig.2 Chromatograms of Nucleotides Peak Asymmetry Peak 1 Peak 2 1.39 1.14 5.10 1.49 Instrument Column Mobile Phase Flow Rate : Shimadzu Nexera : Mastro TM C18(100 mml. 2.1 mmi.d., 3 µm) Typical C18 (100 mml. 2.1 mmi.d., 3 µm) : 10 mm Ammonium Formate in Water : MeCN=99:1 : 0.2 ml/min Column Temp. : 40 Detection : SPD-M20A at (254 nm) Injection Vol. : 1 µl Fig.3
Fig.4 Chromatograms of Sugar Phospahates and Nucleotides Instruments : Shimadzu Nexera/LCMS-8050 Column : Mastro SP (2.1 mmi.d X 100 mml.,5 μm) Mobile phase A : 10 mm Ammonium acetate/mecn=90/10 B : 50 mm Ammonium acetate/mecn=80/20 Gradient B conc. : 0% B (0-4.0 min) 60% B (9.0 min) 100%B (11.0-20.0 min) 0%B (20.1-25.0 min) Oven Temp. : 40 Injection vol. : 3 µl Sample : 2.5 µm STD Mix T.Flow : 0.5 ml/min Nebulizing gas : 3.0 L/min Drying gas : 12 L/min DL Temp. : 250 BH Temp. : 400 Injection vol. : 3 µl セグメント #1 21,873 79,876 210,366 151,006 164,146 170,327 40,854 97,411 69,439 26,920 151,905 26,289 67,224 82,196 57,987 129,243 63,354 193,379 373,078 23,121 24,843 58,584 86,086 47,954 61,741 63,139 173,838 18,372 11,988 28,845 24,690 51,203 31,425 15,237 36,660 6,604 780 10,059 Methionine sulfone 2-Morpholinoethansulfonic acid Glucose 6-phosphate Ribose 5phosphate Sedoheptulose 7-phosphate Fructose 6-phosphate Glycerol 3-phosphate Glucose 1-phosphate Glyceroaldehyde 3-phosphate Erythrose 4-phosphate Ribulose 5-phosphate CMP Dihydroxyacetonephosphate UMP GMP TMP AMP cgmp camp CDP GDP UDP 3-Phosphoglycerate/2-Phosphoglycerate Fructose 1,6-bisphosphate ADP TDP Phosphoenolpyruvate CTP GTP UTP ATP TTP NAD NADP NADH NADPH Succinyl coenzyme A Acetyl coenzyme A 180.10>79.15(-)@1 (1) 194.10>80.15(-)@2 (1) 259.00>97.10(-)@3 (1) 229.00>97.10(-)@4 (1) 289.00>97.10(-)@5 (1) 259.00>97.10(-)@6 (1) 170.90>79.10(-)@7 (1) 258.90>79.10(-)@8 (1) 169.00>97.10(-)@9 (1) 198.90>97.10(-)@10 (1) 229.00>97.10(-)@11 (1) 322.00>79.10(-)@12 (1) 169.00>97.10(-)@13 (1) 322.90>79.10(-)@14 (1) 361.90>79.10(-)@15 (1) 320.90>195.05(-)@16 (1) 346.00>79.10(-)@17 (1) 343.90>150.10(-)@18 (1) 327.90>134.20(-)@19 (1) 402.00>158.90(-)@20 (1) 441.90>159.05(-)@21 (1) 403.00>159.05(-)@22 (1) 185.10>97.10(-)@23 (1) 339.10>97.10(-)@24 (1) 425.90>159.00(-)@25 (1) 401.00>159.00(-)@26 (1) 167.10>79.10(-)@27 (1) 481.90>159.00(-)@28 (1) 521.90>159.00(-)@29 (1) 482.90>159.00(-)@30 (1) 505.90>159.05(-)@31 (1) 481.10>159.00(-)@32 (1) 662.00>539.95(-)@33 (1) 742.20>619.90(-)@34 (1) 664.00>408.00(-)@35 (1) 744.20>408.15(-)@36 (1) 866.00>408.00(-)@37 (1) 808.00>408.00(-)@38 (1) 2.5 5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 25.0 min Fig.5 Chromatograms of Sugar Phospahates and Nucleotides Instruments : Shimadzu Nexera/LCMS-8050 Column : Mastro SP (2.1 mmi.d.x 100 mml.,5 µm) Mobile phase A : 10 mm NH4HCO3/ MeCN=90/10 B : 20 mm NH4HCO3/ MeCN=70/30 Gradient B conc. : 0% (0-3 min) 100% (13.0-20.0 min) 0% (20.1-25.0 min) Oven Temp. : 40 Injection vol. : 2 µl Sample : 2.5 µm STD Mix Nebulizer Gas : 2.0 L/min Drying Gas : 10 L/min Heating Gas : 10 L/min Interface Temp. : 300 DL Temp. : 250 HB Temp. : 400 Dwell Time : 10 ms Pause Time : 1 ms Ionization mode : ESI/negative 注 ) アルカリ条件下での参考アプリケーションです 同条件での使 は カラムの許容 ph 範囲を超える為寿命が短くなりますので 予めご留意ください
3-ADON 15-ADON Fig.6 Chromatograms of 3-ADON/15-ADON,FB1 and FB2/FB3 using Mastro PFP,C18 and Typical PFP columns
NIV DON FUX NEO 15-ADON 3-ADON DAS HT-2 FB1 β-zal α-zal T-2 FB3 FB2 β-zel α-zel ZEN Fig.7 Chromatograms of 17 Mycotoxins Instruments Column : Nexera/LCMS-8060 : Mastro PFP (2.1 mmi.d.x 100 mml., 3 µm) Time program: B20%(0min)-40%(1-1.5min)-50%(1.51-5.5min) -65%(5.51min)-70%(9.5min)-95%(9.51-12min) Flow : 0.3 ml/min Mobile phase A: 10 mm Ammonium acetate in Water B: 2% Acetic acid in MeOH Sample : 50 ng/ml STD Mix