Lipids ON HPLC COLUMNS

Transcription

1 Lipids N HPLC CLUMNS

2 No.TI17E cis - trans Isomers of 9-octadecenoic acid mau min Cadenza CD-C18, 15 x 4.6 mm ACN / water / formic acid = 9 / 1 /.5.8 ml/min, 37 C UV at 215 nm, 3.7 MPa 1 oleic acid CH 2 elaidic acid CH TI17E-AA19

3 No.TI26E live il 15 extra virgin 1 mau min 15 pure 1 mau 5 Cadenza CD-C18 75 x 4.6 mm A : water / formic acid = 1 /.2 B : acetonitrile / formic acid = 1/.2 8-1%B (-1min) 1%B (1-15min) 1. ml/min, 37 C UV at 21 nm, 2.1 MPa min TI26E-AB9

4 No.TI35E Triglycerides in Cacao Butter.18 RI ml/min Minutes Conventional DS (5 um), (25 x 4.6 mm) x 2.6 RI ml/min Minutes acetone / acetonitrile = 7 / 3 3 C RI TI35E-AD25

5 No.TI36E Triglycerides in Linseed il.35.6 ml/min Minutes Conventional DS (5 um), (25 x 4.6 mm) x ml/min Minutes acetone / acetonitrile = 7 / 3 3 C RI TI36E-AD25

6 No.TI37E Triglycerides in Milk Fat ml/min Minutes Conventional DS (5 um), (25 x 4.6 mm) x ml/min Minutes acetone / acetonitrile = 7 / 3 3 C RI TI37E-AD25

7 No.TI38E Triglycerides in Palm il.18.6 ml/min Minutes Conventional DS (5 um), (25 x 4.6 mm) x ml/min Minutes acetone / acetonitrile = 7 / 3 3 C RI TI38E-AD25

8 No.TI41E Lecithin, from Soybeans 1 75 mau min Cadenza CD-C18, 25 x 4.6 mm A : ethanol / water / TFA = 9 / 1 /.1 B : cyclohexane / ethanol / TFA = 1 / 9 /.1 5-1%B ( -1 min ), 1%B ( 1-15 min).5 ml/min, 37 C, 13.9 MPa, UV at 21 nm TI41E-AE31

9 No.TI5E Lavender il 2 mau min 8 Cadenza CD-C18, 25 x 4.6 mm A:.1% formic acid in water B:.1% formic acid in ACN 1-1%B (-7min), 1%B (7-8min) 1. ml/min UV at 254 nm TI5E-AG14

10 No.TI95E Purified Fish il including DHA Glycerides INCRMEGA DHA-J 46 1 mau min INCRMEGA DHA-J 27 1 mau min Cadenza CD-C18, 25 x 4.6 mm acetonitrile / acetone = 7 / 3, 1. ml/min, 37 C, 22 nm Courtesy of Tsuji, Croda Japan TI95E-BJ2

11 No.TI127E Fatty Acid ADAM Derivatives ADAM: 9-anthryldiazomethane C6 Unison UK-C8 3um, 15 x 4.6 mm C6 C8 caproic acid n-hexanoic acid caprylic acid n-octanoic acid C8 C9 C1 C12 C18:3 C14 C18:2 C15 C16 C18:1 C18 C19 C2 C9 C1 C12 pelargonic acid n-nonanoic acid capric acid n-decanoic acid lauric acid n-dodecanoic acid min 4 BRAND-M 5um, 25 x 4.6 mm C18:3 alpha-linolenic acid cis-9,12,15-octadecatrienoic acid C14 myristic acid n-tetradecanoic acid C18:2 linoleic acid cis-9,12-octadecadienoic acid. -.5 C15 pentadecanoic acid n-pentadecanoic aci C16 palmitic acid n-hexadecanoic acid C18:1 oleic acid cis-9-octadecenoic acid C18 stearic acid n-octadecanoic acid min C19 nonadecanoic acid n-nonadecanoic acid Unison UK-C8, 15 x 4.6 mm water / acetonitrile = 15 / 85, 1. ml/min, 3 C FLS Ex365 nm, Em412 nm C2 arachidic acid eicosanoic acid TI127E-CH12

12 No.TI135E Volicitin-related Compounds from the ral Secretion of Caterpillars 1 3 MS UV R 3 4 R' R = H, R = H, 1 3 HC NH CNH2 5 6 R' = H, 2 R' = H, 4 HC NH CNH2 R Cadenza CD-C18, 75 x 3 mm A:.5% acetic acid in water B:.8% acetic acid in acetonitrile 2-95%B ( -4min ).2 ml/min, 6 C, 1 µl Negative ESI mass, UV at 2 nm R = H, 5 R = H, 7 6 H H Courtesy of Dr. Naoki Mori, Kyoto Univ. TI135E-CG25

13 No.TI244E Monoglycerides 1 H C H CH2 CH CH2 2-oleoylglycerol H CH2 2 H C H CH CH2 CH2 1-oleoylglycerol (monoolein) 3 H C CH CH2 monoelaidin 2 mau min 75 x 4.6 mm, water / acetonitrile = 1 / 9 1 ml/min, 37 degc, 21 nm, 5 ul (2.5 ug) TI244E-EG4

14 No.TI331E Fatty Acids CH3(CH2)nCH lauric acid (n=1) 2. myristic acid (n=12) 3. palmitic acid (n=14) 4. stearic acid (n=16) 5. arachidic acid (n=18) mv 5 3 normal phase min Unison UK-Amino, 25 x 3 mm acetonitrile / 1mM ammonium acetate = 9 /1.4mL/min (6 MPa), 5deg.C ELSD,.5uL (.6-3ug) mv reversed phase min Cadenza CD-C18, 25 x 3 mm A: water /formic acid = 1 /.1 B: acetonitrile / THF / formic acid = 5 / 5 / %B (-2min).4mL/min (12 MPa), 37deg.C ELSD,.7uL (.8-4ug) TI331E-GH3

15 No.TI354E Essential il (Peppermint) 246 peaks mau %B(-24min), 1%B(24-3min), 16MPa, 2uL min 169 peaks mau %B(-12min), 1%B(12-15min), 9MPa, 1uL min Cadenza CD-C18 A: water / trifluoroacetic acid = 1 /.1 B: acetonitrile / trifluoroacetic acid = 1 /.1.5mL/min, room temp., 22 nm TI354E-GH7

16 No.TI355E Essential ils mau 2 peppermint 246 peaks 15 sandalwood 153 peaks 1 eucalyptus 168 peaks grapefruit 142 peaks 5 lavender 146 peaks min Cadenza CD-C18, 5 x 4.6 mm A: water / trifluoroacetic acid = 1 /.1 B: acetonitrile / trifluoroacetic acid = 1 /.1 4-1%B(-24min), 1%B(24-3min).5mL/min (16MPa), room temp., 22 nm, 2uL TI355E-GH8

17 No.TI477E LC-MS application for phospholipids 1 % 1 % :/2:4-PI :/18:1-PC 2 1: TF MS ES e3 1: TF MS ES e4 CH2CR1 R2 CCH CH2 P Phosphatidylinositol (PI) H H H H H 1 % :/18:2-PC 3 1: TF MS ES e3 CH2CR1 R2 CCH CH2 P Phosphatidylcholine (PC) CH2CH2N(CH3)3 1 % 1 % 1 % 1 % Fused Core TM 1: TF MS ES e4 1: TF MS ES e4 1: TF MS ES- TIC 1.4e a 4.19 b :1/18:1-PE (2.7um), DS, 1 x 2.1 mm Time 1: TF MS ES TIC TIC, 5 x 1 4 FS 5.5e a 16:/18:1-PG b d18:1/c16:-sm 5 6 TIC, 1 x 1 5 FS CH2CR1 R2 CCH CH2 P Phosphatidylethanolamine (PE) CH2CH2NH3 CH2CR1 R2 CCH CH2 P H H CH2CHCH2 H Phosphatidylglycerol (PG) CH R1 R2CNH CH CH2 P CH2CH2N(CH3)3 Sphingomyelin (SM) Scan Cadenza CW-C18, 1 x 2 mm 5mM HCNH4 in (acetonitrile / methanol = 1 / 1).2mL/min, 2deg.C ESI-TFMS, Negative Courtesy of Yasuko Yoshioka, Inst. Health Biosciences, Univ. of Tokushima, Japan TI477E-IA8

18 No.TI487E LC-MS/MS Application for Sphingolipids (Ceramide) XIC of +EMS: to amu from Sample 1 (C16 Ceramide) of March_11_9_p... Max. 3.3e8 cps. 3.3e8 3.e8 2.5e8 H NH 16: Ceramide (C16 Ceramide) N-Palmitoylsphingosine H e8 1.5e8 +EMS: to min from Sample 1 (C16 Ceramide) of March_11_9_pos_EM e6 9.e6 8.e6 7.e6 6.e Max. 9.6e6 cps. 5.e e8 5.e7. 4.e6 3.e6 2.e6 1.e m/z, amu Time, min Cadenza CW-C18, 15 x 2 mm A: [water / HCH (1:.2 v/v)] containing 7mM ammonium formate B: [methanol / HCH (1:.2 v/v)] containing 5mM ammonium formate 7-9%B (-1min), 9%B (1-1.5min), 9-1%B ( min), 1%B (2.5-6min), 1-4%B (6-6.5min), 4%B (6.5-1min).2mL/min -.28mL/min (-6min),.2mL/min (6-1min) 48deg.C, 5uL (5ug / ml) Applied Biosystems QTrap, ESI Positive [M-H2+H] Courtesy of Jennifer Ro and Joe Williams Department of Evolution, Ecology, and rganismal Biology, hio State University - USA TI487E-IC2

19 No.TI488E LC-MS/MS Application for Sphingolipids (Sphinganine) XIC of +EMS: 32. to 34.9 amu from Sample 1 (sphinganine) of March_11_9_pos... Max. 2.3e8 cps. 2.3e8 2.2e8 2.e Sphinganine (Dihydrosphingosine) H NH2 H 1.8e8 1.6e8 1.4e8 1.2e8 1.e8 8.e7 +EMS: to min from Sample 1 (sphinganine) of March_11_9_pos_EMS_ e6 3.e6 2.5e6 2.e6 1.5e6 6.e7 1.e e7 2.e e m/z, amu Time, min Cadenza CW-C18, 15 x 2 mm A: [water / HCH (1:.2 v/v)] containing 7mM ammonium formate B: [methanol / HCH (1:.2 v/v)] containing 5mM ammonium formate 7-9%B (-1min), 9%B (1-1.5min), 9-1%B ( min), 1%B (2.5-6min), 1-4%B (6-6.5min), 4%B (6.5-1min).2mL/min -.28mL/min (-6min),.2mL/min (6-1min) 48deg.C, 5uL (5ug / ml) Applied Biosystems QTrap, ESI Positive Courtesy of Jennifer Ro and Joe Williams Department of Evolution, Ecology, and rganismal Biology, hio State University - USA TI488E-IC2

20 No.TI489E LC-MS/MS Application for Sphingolipids (Sphingosine) XIC of +EMS: to amu from Sample 1 (sphingosine) of March_11_9_pos... Max. 3.e8 cps. 3.e8 2.5e Sphingosine H NH2 H 2.e8 +EMS: to min from Sample 1 (sphingosine) of March_11_9_pos_EMS_... 3.e Max. 3.1e6 cps. 1.5e8 2.5e6 2.e6 1.e8 1.5e6 1.e e e m/z, amu Time, min Cadenza CW-C18, 15 x 2 mm A: [water / HCH (1:.2 v/v)] containing 7mM ammonium formate B: [methanol / HCH (1:.2 v/v)] containing 5mM ammonium formate 7-9%B (-1min), 9%B (1-1.5min), 9-1%B ( min), 1%B (2.5-6min), 1-4%B (6-6.5min), 4%B (6.5-1min).2mL/min -.28mL/min (-6min),.2mL/min (6-1min) 48deg.C, 5uL (5ug / ml) Applied Biosystems QTrap, ESI Positive [M-H2+H] Courtesy of Jennifer Ro and Joe Williams Department of Evolution, Ecology, and rganismal Biology, hio State University - USA TI489E-IC2

21 No.TI49E LC-MS/MS Application for Sphingolipids (Sphingosine-1-P4) XIC of -EMS: to 38.9 amu from Sample 1 (S1P) of March_13_9_neg_EMS_... Max. 1.5e6 cps. 1.5e6 1.4e6 1.2e6 1.e6 8.e5 6.e5 4.e EMS: to min from Sample 1 (S1P) of March_13_9_neg_EMS_S1P.wiff e4 2.4e4 2.2e4 2.e4 1.8e4 1.6e4 1.4e4 1.2e4 1.e H Max. 2.7e4 cps m/z, amu P + NH3 H Sphingosine-1-Phosphate 2.e Time, min Cadenza CW-C18, 15 x 2 mm A: [water / HCH (1:.2 v/v)] containing 7mM ammonium formate B: [methanol / HCH (1:.2 v/v)] containing 5mM ammonium formate 7-9%B (-1min), 9%B (1-1.5min), 9-1%B ( min), 1%B (2.5-6min), 1-4%B (6-6.5min), 4%B (6.5-1min).2mL/min -.28mL/min (-6min),.2mL/min (6-1min) 48deg.C, 5uL (3ug / ml) Applied Biosystems QTrap, ESI Negative Courtesy of Jennifer Ro and Joe Williams Department of Evolution, Ecology, and rganismal Biology, hio State University - USA TI49E-IC2

22 No.TI491E LC-MS/MS Application for Sphingolipids (Sphinganine-1-P4) XIC of -EMS: to amu from Sample 2 (dhs1p) of March_13_9_neg_EMS... Max. 4.6e6 cps. 4.5e6 4.e6 3.5e6 3.e6 2.5e6 2.e6 1.5e6 1.e6 5.e EMS: to 4.86 min from Sample 2 (dhs1p) of March_13_9_neg_EMS_S1P m/z, amu Time, min 1.4e5 1.2e5 1.e5 8.e4 6.e4 4.e4 2.e4 H 38.4 P + NH3 H Sphinganine-1-Phosphate (Dihydrosphingosine-1-phosphate) Cadenza CW-C18, 15 x 2 mm A: [water / HCH (1:.2 v/v)] containing 7mM ammonium formate B: [methanol / HCH (1:.2 v/v)] containing 5mM ammonium formate 7-9%B (-1min), 9%B (1-1.5min), 9-1%B ( min), 1%B (2.5-6min), 1-4%B (6-6.5min), 4%B (6.5-1min).2mL/min -.28mL/min (-6min),.2mL/min (6-1min) 48deg.C, 5uL (5ug / ml) Applied Biosystems QTrap, ESI Negative Courtesy of Jennifer Ro and Joe Williams Department of Evolution, Ecology, and rganismal Biology, hio State University - USA TI491E-IC2

23 No.TI562E Lipopolysaccharide (from E.coli 127) mv min Presto FF-C18, 5 x 4.6 mm A: water / formic acid = 1 /.1 B: acetonitrile / formic acid = 1 /.1-7 %B (-5 min).5 ml/min (7 MPa), 37 deg.c ELSD (spray chamber 3 deg.c, drift tube 8 deg.c) 5 ul (1 ug) mv min Presto FF-C18, 15 x 4.6 mm A: water / formic acid = 1 /.1 B: acetonitrile / formic acid = 1 /.1-7 %B (-25 min).2 ml/min (7 MPa), 37 deg.c ELSD (spray chamber 3 deg.c, drift tube 8 deg.c) 5 ul (1 ug) Imtakt USA (info@imtaktusa.com) North America Imtakt Corp./JAPAN (info@imtakt.com) ther Countries TI562E-JA18