1 WSV SIR m/z Analyte RT (Min) SIR m/z Cone voltage (V) Ascorbic Acid (C) Thiamine (B1) Nicotinic Acid (B3) Pyridoxal (
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1 ACQUITY UPLC H-Class ACQUITY QDa Mark E. Benvenuti, Dimple Shah, and Jennifer A. Burgess Waters Corporation, Milford, MA, USA MS ACQUITY QDa UPLC HPLC UV ACQUITY QDa LC EC 1925/26 CFR 21 HPLC 1 LC-MS ACQUITY QDa 12 WSV ACQUITY UPLC H-Class ACQUITY UPLC QDa ACQUITY UPLC H-Class ACQUITY QDa WSV QDa 1
2 1 WSV SIR m/z Analyte RT (Min) SIR m/z Cone voltage (V) Ascorbic Acid (C) Thiamine (B1) Nicotinic Acid (B3) Pyridoxal (B6) Nicotinamide (B3) Pyridoxine (B6) Ca_Pantothenate (B5) Cyanocobalamin (B12) Folic Acid (B9) B2-5-Phosphate Biotin (B7) Riboflavin (B2) SIR Standard Individual B complex vitamins (mg/l ) Vitamin C (mg/l) WSV 1 mg/ml B2 B7 B9 98 µl 1N NaOH 2 µl C ph3.2 C 1.25 ml 25 ml 25 ml C 5 ppm 1 ppm g 1 ml.2 µm PVDF g 1 ml 15.2 µm PVDF µm PVDF 2. B C 2
3 UPLC LC ACQUITY UPLC H-Class 17.5 ACQUITY UPLC HSS T3 1.8 µm mm A 1 mm.1 B 1 mm.1 5 µl A B ml/ 1. Initial ACQUITY UPLC PDA 21~4 nm 27 nm 1 / 2 ACQUITY QDa ESI kv MS 5~8 m/z SIR 5 Hz 15 V 1 SIR SIR m/z 2 3 3
4 MS m/z 2 2 D F m/z=442 m/z =678 2 UV 2A 2H UV 3 MS Ascorbic Acid C 2- Thiamine B1 3- Nicotinic acid B3 4- Pyridoxal B6 5- Nicotinamide B3 6- Pyridoxine B6 7- Ca_Pantothenate B5 8- Cyanocobalamin B12 9- Folic acid B9 1- Riboflavin 5 phosphate 11- Biotin B7 12- Riboflavin B SIR 4
5 Compound name: Biotin (B7) Correlation coefficient: r = , r 2 = Calibration curve: * x type: External Std, Area A Compound name: Thiamine (B1) Correlation coefficient: r =.99633, r 2 = Calibration curve: * x type: External Std, Area B Compound name: Riboflavin (B2) Correlation coefficient: r = , r 2 = Calibration curve: * x type: External Std, Area C Compound name: Folic Acid (B9) Correlation coefficient: r = , r 2 = Calibration curve: * x type: External Std, Area D Compound name: Riboflavin 5 phosphate Correlation coefficient: r = , r 2 = Calibration curve: * x type: External Std, Area E Compound name: Cyanocobalamin ( B12) Correlation coefficient: r = , r 2 = Calibration curve: * x type: External Std, Area F Conc Compound name: Nicotinic Acid (B3) Coefficient of Determination: r 2 = Calibration curve: * x * x type: External Std, Area Curve type: 2nd Order, Origin: Exclude, Weighting: 1/x, Axis trans: None G Compound name: Ca_Pantothenate (B5) Correlation coefficient: r = , r 2 = Calibration curve: * x type: External Std, Area H
6 MS UV µg/l SIR UV 3A 27 nm 3A UV MS 5.e-4 A: UV at 27 nm RT 2.46, S/N = 63 B: Pyridoxine SIR m/z RT 1.75, S/N = 32 C: Pyridoxal SIR m/z RT 1.24, S/N = 19 D: Nicotinic Acid SIR m/z RT 2.43, S/N = 33 E: Nicotinamide SIR m/z Time µg/ml 27 nm UV SIR SIR 4 B C D E 6
7 4 2 B5 UV UV B1 UV 1 5 B1 C C UV B1 5A ACQUITY QDa SIR B1 A B C MS Vitamin water 1 PDA Vitamin water 1 MS Vitamin water 2 7: SIR of 1 Channel ES+ 242 (Ca_Pantothenate (B5)) 14: Diode Array 7: SIR of 1 Channel ES+ 242 (Ca_Pantothenate (B5)) D 2. PDA Vitamin water 2 14: Diode Array Time 4. 2 B5 5.9 MS A C UV B D 1 Thiamine, 1.1 RT 1.1 A: SIR of thiamine (B1) Ascorbic acid,.91 RT.91 B: SIR of ascorbic acid(c) e-1 Ascorbic acid,.9 RT.9 C: UV at 27 nm 1.e Time A B1 SIR B C SIR C C 27 nm UV B1 UV 7
8 2 4 UPLC 6 UV 6B B12 ACQUITY QDa LC A: SIR of cyanocobalamin : SIR of 1 Channel ES+ 678 (Cyanocobalamin (B12) B: UV at 27 nm (1) PDA Ch1 27 nm at 1.2 nm 1.e-2 8.e-3 6.e-3 4.e-3 2.e-3 Time B12 A UV B 8
9 1 6 µg B12 16 mg B3 LC-MS 7 7A 7B B2 1 SIR 7C B12 SIR 27 nm UV 7D 12.5 ppm A 1 Diluted x SIR at m/z 377 Riboflavin (B2) B Undiluted 7.71 SIR at m/z 377 Riboflavin (B2) C 1 Undiluted SIR at m/z 678 Cyanocobalamin (B12) D UV at 27nm 2.e-1 Undiluted 1.e Time A B12 C B UV D 9
10 B RSD=.6 25 mg/l RSD=1 Analyte RSD for retention time Thiamine (B1).6 Nicotinic Acid (B3).19 Pyridoxal (B6).23 Nicotinamide (B3).22 Pyridoxine (B6).26 Ca_Pantothenate (B5) 4 Cyanocobalamin ( B12) 3 Folic Acid (B9) 3 Riboflavin 5 phosphate 3 Biotin (B7) 2 Riboflavin (B2) mg/l 1 25 mg/l 1 Analyte RSD for area Thiamine (B1) 6.78 Nicotinic Acid (B3) 2.35 Pyridoxal (B6) 2.62 Nicotinamide (B3) 2.24 Pyridoxine (B6) 2.65 Ca_Pantothenate (B5) 4.6 Cyanocobalamin ( B12) 7. Folic Acid (B9) Riboflavin 5 phosphate Biotin (B7) 2.77 Riboflavin (B2) mg/l 1 B 1
11 UV ACQUITY QDa SIR ACQUITY QDa 1. G F M Ball (Editor). Bioavailabilty and Analysis of Vitamins in Foods. Chapman and Hall. (1998). Ch2, pp E Riches. The Rapid Simultaneous Analysis of 12 Water Soluble Vitamin Compounds. Waters Application Note No en, June, Heudi et al. Separation of water-soluble vitamins by reversed-phase high performance liquid chromatography with ultra-violet detection: Application to polyvitaminated premixes. J Chrom A. (25) 17: 49 56, pp AOAC Method 211.9: Vitamin B12 in Infant Formula and Adult Nutritionals. (212). UV LC-MS Empower 3 Mass Lynx 2 LC ACQUITY QDa TEL FAX F TEL FAX Waters ACQUITY UPLC UPLC Empower MassLynx QDa T he Science of What s Possible Waters Corporation 214 Waters Corporation. Printed in Japan JA PDF
FOOD TESTING ACQUITY QDa Simplify matrix complexity and extend detection capabilities
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島津ジーエルシー総合カタログ2017【HPLCカラム】
56 Shimadzu GLC Ltd.H Luna R 社独自の技術をもとに 優れた ph 安定性と再現性を持つ逆相系カラムです ph1.5-9.0( ) の ph 領域において 酸性 塩基性および両性化合物の分析が可能です ph1.5-9.0( ) の領域において 1,000 時間以上安定してお使いいただけます 多種の粒子径やカラムサイズ 固定相を取り揃えております ガードカラムを除くすべてのカラムに基材品質保証書
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Mastro -リン酸基含有化合物分析に対する新規高耐圧ステンレスフリーカラムの有用性について-
学会発表資料 _ 抜粋 リン酸基含有化合物分析に対する新規高耐圧ステンレスフリーカラムの有用性について 佐藤友紀 1,3, 山口忠行 2, 尾坂裕輔 2, 山本祝久 1 ( 株式会社島津ジーエルシー 1, 株式会社島津製作所 2, 独立行政法人国立循環器病研究センター薬剤部 3) はじめに リン酸基含有化合物や 属キレート性のある化合物は, 分析を う際にテーリング現象や吸着現象が起こる事が一般的に知られている
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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
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2,4-2,4-Dimethylaniline 2,4-2,4-Xylidine CH 3 CH 3 CAS 95-68-1 C 8 H 11 N 121.18 121.0892-14.3 C 2) 214 C 2) 0.9723 g/cm 3 2) 0.133 mmhg (25 C) 1) 1390 mg/l (25 C) 1) 3.710 3 mg/l 25 C WSKOWWIN 5) 6.0710
GPC/SEC... 3 GPC... 4 GPC... 5 Agilent PL-SP 260VS... 6 Agilent PL-GPC 220 GPC/SEC... 7 Agilent Cirrus GPC GPC... 9... 10 GPC/SEC... 11 GPC Agilent PL
GPC/SEC Greg Saunders Ben MacCreath GPC/SEC... 3 GPC... 4 GPC... 5 Agilent PL-SP 260VS... 6 Agilent PL-GPC 220 GPC/SEC... 7 Agilent Cirrus GPC GPC... 9... 10 GPC/SEC... 11 GPC Agilent PLgel Olexis... 12...
(EQP) (DQ) (IQ) (OQ) OQ (RQ) IQ OQ IQ OQ (ACE) OQ EQP EQP Adobe (i) Q & A (ii) Agilent Compliance Engine (ACE) - 21 CFR Part11 (iii) EE 1.76 EQR 3 PDF
Equipment Qualification Plan (EQP) GC Agilent 7890/7820 (CTC ) Agilent 6890/6850/5890 GC EQP : Agilent_Recommended_EQP_GC (EQP) (DQ) (IQ) (OQ) OQ (RQ) IQ OQ IQ OQ (ACE) OQ EQP EQP Adobe (i) Q & A (ii)
14 12 10 8 6 4 2 0 1 2 3 4 5 6 7 8 9 10 11 12 20 0 0 0 0 0 0 0 0 0 0 0 0 21 0 0 0 0 0 0 0 0 0 0 0 0 22 0 0 0 0 0 0 0 0 0 0 0 0 23 0 0 0 0 0 0 0 0 0 0 0 0 24 0 0 0 0 0 0 0 0 0 0 0 0 25 0 0 0 0 0 0 0 0 0
Agilent BioHPLC HPLC/UHPLC /
Agilent BioHPLC HPLC/UHPLC / HPLC/UHPLC ( Å Å ) BioHPLC MPa.. µm UHPLC Poroshell ( ) Agilent AdvanceBio RP-mAb : AdvanceBio RP-mAb Poroshell mab Agilent AdvanceBio :.7 µm C AdvanceBio Agilent Poroshell
a b Chroma Graphein Chromatography
a b Chroma Graphein Chromatography (Stationary Phase) (Mobile Phase) CHROMATOGRAPHY GAS SFC LIQUID GSC GLC Column Planar NP RP IEC SEC TLC Paper Normal Phase Reverse Phase GPC GFC Thin Layer Chromato.
PC LC8 TLSXB92JC (%) 5 15 25 3 35 (h) : D-SUB : RS-232C WORLD-WIDE OPERATION 142 227 311 142 227 311 (%) 9 7 5 3 1 : LC8 : A14-5-11 5 mm1 m 1 3 5 (%) 142 227 311 142 227 311 TLSXB143JB 7 9 mm TLSXB144JB
0.1 IEC 60598 1,000 IEC 60598-2 1,000V CIE 11.2 IEC 60598-2 IEC 60598-1 - 1 - IEC IEC 0.2 IEC 60598-1 IEC 60598-1 IEC ISO IEC 60061-2 IEC 60061-3 IEC 60065 1969 1995 1969 1995 1985 IEC 60068-2-63 1991