MACHEREY-NAGEL Chromatography Based on core-shell technology nenhanced π-π interactions and remarkable efficiency nexcellent stability in 00 % aqueous mobile phase nsuitable for LC/MS due to low bleeding characteristics
Key features n Special biphenylpropyl core-shell phase with multi-endcapping n Separation mode based on two retention mechanisms: π-π interactions and hydrophobic interactions n Enhanced retention for aromatic and unsaturated substances n Excellent performance under highly aqueous conditions n Suitable for LC/MS due to low bleeding characteristics n Higher hydrophobcity in comparison to other aryl phases Recommended Applications n Overall sophisticated analytical separations n Aromatic and unsaturated compounds n Mycotoxins n Phthalates n Pesticides n Antibiotics n Hormones n Pharmaceuticals n DNPH Aldehydes USP L Similar phases: Kinetex Biphenyl, Raptor Biphenyl, HALO Biphenyl Technical data Biphenylpropyl modification with multi-endcapping on core-shell particles ph stability:.5 8.5 Particle size: Pore size:.7 µm (core.7 µm) 90 Å Specific surface: 0 m /g Carbon content: 5. % NUCLEOSHELL Biphenyl Si Si TMS Batch-to-batch reproducibility MN Appl. No. 8760 MN REF: 766.40 EC 50/4,.7 μm 5 mm potassium dihydrogen phosphate solution methanol (70:0, v/v), ph = 7.0 Run time:.0 ml/min 0 min Temperature: 0 C UV, 54 nm μl (in methanol) Uracil 40 µg/ml (void volume marker) Toluene 50 µg/ml Ethylbenzene 50 µg/ml Lidocaine 500 µg/ml Acenaphthene 0 µg/ml Batch Batch Batch Batch 4 Batch 5 Excellent reproducibility High batch-to-batch reproducibility of columns show reliable results for different LOTs. k' Toluene k' Ethylbenzene k' Lidocaine k' Acenaphthene
Stability in 00 % aqueous eluent MN Appl. No. 8770 MN REF: 7664.0 Run time: EC 00/,.7 μm 0 mm potassium dihydrogen phosphate solution, ph =. isocratic 0.56 ml/min 0 min Temperature: 0 C Test mix: UV, 0 nm and 54 nm 0.5 μl Cytosine, Uracil, Thymine in water Retention time [min] 4.5 4.5.5.5 0.5 RT Cytosin RT Uracil RT Thymine 0 50 00 50 00 50 00 50 400 Number of injections 00 % aqueous stability Excellent performance and ruggedness using 00 % aqueous mobile phase. Stability in acidic medium (isocratic method) MN Appl. No. 8790 EC 00/,.7 μm MN REF: 7664.0 acetonitrile water (60:40, v/v), % TFA (ph = 0.8) isocratic 0.56 ml/min Run time: 0 min Temperature: 60 C UV, 54 nm 0. µl Test mix: Uracil, Biphenyl, Anthracene in acetonitrile Retention time [min].5 Uracil Biphenyl Anthracene.5.5 0.5 0 50 00 50 00 50 00 50 400 Number of injections Stability in acidic medium (gradient method) MN Appl. No. 8780 MN REF: 7664.0 EC 00/,.7 μm A) % H PO 4 (ph =.) B) acetonitrile Temperature: 40 C equilibration 0 min 0 % B, hold 0 % B for 5 min, from 0 % to 90 % B in 5 min, hold 90 % B for min, in.0 min to 0 % B 0.56 ml/min UV, 54 nm.,.7 µm. Kinetex Biphenyl,.6 µm. Raptor Biphenyl,.7 µm Chromatogram Absorbance [mau] 80 60 40 0 0-0 5.00 6.5 7.50 8.75 0.00 min Enhanced stability at low ph values Very low bleeding characteristic in UV-VIS measurements compared to other core-shell biphenyl phases in acidic medium.
Disperse dyes MN Appl. No. 8800 MN REF: 7664.0 Temperature: 0 C EC 00/,.7 μm A) 0. % formic acid in water B) 0. % formic acid in acetonitrile hold 5 % B for.0 min, in 6.0 min to 95 % B, hold 95 % B for.0 min, in 0. min to 5 % B, hold 5 % B for 4.9 min 0.56 ml/min MS, SMRM μl 0 ng/ml for each analyte in water Chromatograms Intensity [cps] 8.0e6 7.0e6 6.0e6 5.0e6 4.0e6.0e6.0e6.0e6 MRM transitions Analyte Polarity RT [min] [M+H] + Q (Quantifier) Q (Qualifier) Basic Red 9 positive 5.0 88. 95.0 67.0 Disperse Blue positive 6. 97. 8.0 5.0 Disperse Red positive 6. 68.0 4.9 5.9 Basic Violet positive 6. 58. 4. 6. Disperse Yellow 9 positive 6.4 75. 9.9 8.0 Disperse Blue 0 positive 6.4 66. 08.0 47. Disperse Red 7 positive 6.5 45. 64.0 77.0 Crystal Violet positive 6.7 7. 56. 40. Disperse Yellow 9 positive 6.7 65. 49.0 50.0 Disperse Yellow positive 6.9 70. 07. 08. Disperse Blue 06 positive 6.9 6. 78. 47.0 Victoria Blue B positive 7. 470. 454. 49. Disperse Orange positive 7. 4..0 75. Disperse Brown positive 7. 4.0 97.0 57.0 Disperse Blue 5 positive 7.5 85. 70.0 9.9 Disperse Blue 4 positive 7.6 78. 0.0 87. Disperse Yellow 49 positive 7.6 75. 8..0 Disperse Orange positive 7.7 8..9 65.0 Disperse Yellow positive 7.9 0. 77. 05. Disperse Blue positive 8. 69. 7.0 6. Disperse Blue 6 positive 8. 99. 8.9 67. Disperse Orange positive 8. 9. 69.0.0 Disperse Orange 7 positive 8. 9. 5.0. Analyte Polarity RT [min] [M-H] Q (Quantifier) Q (Qualifier) Disperse Yellow negative 6.8 74.0 44.0 7.0 Disperse Orange 49 negative 8.7 457. 65.9.0 Intensity [cps].0e6 9.0e5 8.0e5 7.0e5 6.0e5 5.0e5 4.0e5.0e5.0e5.0e5 0.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 min 0.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 min 4
Mycotoxins MN Appl. No. 880 MN REF: 7664.0 EC 00/,.7 μm A) 0. % formic acid in water B) 0. % formic acid in acetonitrile hold 5 % B for.0 min, in.0 min to 40 % B, in.0 min to 95 % B, hold 95 % B for.0 min, in.0 min to 5 % B, hold 5 % B for.0 min Temperature: 40 C 0.56 ml/min MS, SMRM 0 μl 0.5 ng/ml fumonisin B in water, 5.0 ng/ml for each other analyte in water MRM transitions Chromatogram Intensity [cps].0e6.8e6.6e6.4e6.e6.0e6 0.8e5 0.6e5 0.4e5 0.e5 0.0.6.8 4.0 4. 4.4 4.6 4.8 5.0 5. 5.4 5.6 min Analyte RT [min] [M+H] + Q (Quantifier) Q (Qualifier) Fumonisin B 4.55 7. 4. 5. Fumonisin B 5.00 706. 6. 8. HT- toxin 5. 45. 6.0 5.0 Afl atoxin G 5.0..0 44.9 Afl atoxin B 5..0 85.0 4.0 Afl atoxin G 5.4 9.0 4.9.0 Afl atoxin B 5.46 5. 87.0 58.9 T- toxin 5.5 467. 05.0 44.9 Deoxynivalenol 5.65 97. 80. 48.8 Zearalenone 5.70 9. 87. 85.0 Ochratoxin A 5.7 404.0 8.8 58.0 5
Pesticides MN Appl. No. 880 MN REF: 766.46 Temperature: 0 C EC 50/4.6,.7 μm A) 0. % formic acid in water B) 0. % formic acid in methanol in 5 min from 5 % to 00 % B, hold for.0 min, in 0. min to 5 % B, hold 5 % B for.9 min 0.70 ml/min MS, SMRM 0 μl 0.4 ng/ml in water QuEChERS mix extract (4:, v/v) Sample matrix: g black tea (spiked with 50 µg/kg for each pesticide) Chromatogram 4.0e6.0e6 Intensity [cps].0e6.0e6 0.0 0.5.0.5.0.5.0.5 4.0 4.5 5.0 5.5 6.0 6.5 min Retention times / relative retention times / recovery rates Analyte RT [min] Relative RT [%] Recovery rate [%] Cyromazine 0.98 0. 8 4. Methamidophos.70 8.9 67 0. Aminocarb.07 47.9 78 7. Propamocarb.0 6.5 6 5.8 Formetanate.5 58. 68.5 Omethoate.0 9. 8 5. Pymetrozine. 5.0 8 7.0 Aldicarb sulfoxide.49 4.5 88 9. Carbendazim.6 4.4 69 6.4 Aldicarb sulfone.74 9.9 78.6 Nitenpyram.8 5.7 5 4.4 Mexacarbate.90 6. 85. Monocrotophos.00.4 85.7 Flonicamid.0 4.9 8 4.7 Methomyl.0.4 8 4. Fuberidazole.0. 7. Dicrotophos. 8. 80.4 Standard deviation [%] Analyte RT [min] Relative RT [%] Recovery rate [%] Ethirimol.5 5.0 4.8 Fenuron.5 5.8 85 4.9 -Hydroxycarbofuran.56 4.8 87 6. Dimethoate.70 6.7 87. Imidacloprid.86. 8 6.0 Mevinphos isomer.90.7 9.0 Mevinphos isomer.90.7 8 9. Pirimicarb.96 7.5 79.6 Cymoxanil 4.00.0 86. Prometon 4.06 0.5 8.4 Simetryn 4.07.7 8.7 Butocarboxim 4.07 0.8 9 5.7 Carbetamide 4.07 09.7 94 5.5 Aldicarb 4.08 4.9 90 6. Secbumeton 4.09.4 8. Acetamiprid 4. 9.6 88 5. Imazalil 4.9 0. 7 6.8 Standard deviation [%] in relation to NUCLEOSHELL Bluebird RP 8 Continued on page 7 6
Continued from page 6 Analyte RT [min] Relative RT [%] Recovery rate [%] Thidiazuron 4.6 08.7 9 6.7 Bendiocarb 4.4.6 9 4.5 Propoxur 4.5. 84 4. Ametryn 4.4 6. 8.9 Fluometuron 4.4 08.9 95 5.6 Carbofuran 4.4 7.5 95 5.5 Spiroxamine isomer 4.45 6.4 98 5. Spiroxamine isomer 4.45 6.4 07. Carbaryl 4.45 09.9 9 8.4 Fenpropimorph 4.47 5.9 5.7 Metribuzin 4.49 6.6 89 6. Monolinuron 4.5 0.0 9 8.0 Thiophanate-methyl 4.5 7. 46 9. Propham 4.54 07. 75 5. Chlorotoluron 4.55 08. 76 8.8 Isoprocarb 4.57 07.8 86 0. Oxadixyl 4.60 7.8 8 0.7 Methoprotryne 4.60. 84.8 Metobromuron 4.6 0.9 79.7 Forchlorfenuron 4.64 06.7 68 4.4 Isoproturon 4.66 08. 85 9.4 Thiofanox 4.69 5.0 6 8.5 Diuron 4.69 0.0 7.9 Prometryne 4.70 6.6 8 6. Flutriafol 4.7.6 8 4. Desmedipham 4.74 07.7 9.4 Pyrimethanil 4.76.6 8 8. Cycluron 4.77 09.9 89 0.5 Phenmedipham 4.78 0.4 99 6.6 Methabenzthiazuron 4.8.4 8 8.5 Fenobucarb 4.8 09.8 97 9.4 Linuron 4.90 07.0 87 0.4 Diethofencarb 4.9 09.8 87. Promecarb 4.9 06.5 04.7 Halofenozide 4.9 08. 8.8 Hydramethylnon 4.94.8 40 0.8 Metalaxyl 4.97 5.9 89 4.8 Ethiprole 4.97 0.9 87.7 Paclobutrazol 4.99 08.5 88 5.0 Methiocarb 5.00 08.9 94.6 Flutolanil 5.0 08.0 90 6. Chlorantraniliprole 5.0 4. 79 9. Fenamidone 5.05 0.5 8 7. Iprovalicarb isomer 5.06 06. 96 4.4 Iprovalicarb isomer 5.08 06.5 96.6 Nuarimol 5.09.9 6 0.0 Ethofumesate 5..8 66 5.0 Mepronil 5. 08.7 89.7 Methoxyfenozide 5. 08. 9 0.4 Thiacloprid 5. 49.6 8.5 Furalaxyl 5.4.7 89.8 Cyproconazole isomer 5.4 0.5 87 4.5 Cyproconazole isomer 5.4 09.6 90 4.0 Cyprodinil 5.5.0 8 4.0 Boscalid 5.6 4.7 95 0. Chloroxuron 5.6 08.9 84 4.7 Triadimefon 5.8.4 88.0 Bifenazate 5.9 0.4 9 6. Bupirimate 5.0 7.4 86. Tetraconazole 5.0 09.7 0. Mepanipyrim 5.0 07.4 77.5 Neburon 5. 05.7 9.5 Carfentrazone-ethyl 5. 5.7 97. in relation to NUCLEOSHELL Bluebird RP 8 Standard deviation [%] Analyte RT [min] Relative RT [%] Recovery rate [%] Diclobutrazol 5.5 08.9 9. Tebufenozide 5.6 09.4 9.7 Difl ubenzuron 5.7 08.7 90.4 Fenarimol 5..9 89 8.7 Azoxystrobin 5.4 6.8 95 4.5 Tebuconazole 5.5 08. 85 8.4 Hexaconazole 5.5 07.0 9.0 Fenoxycarb 5.6 09. 4.0 Acibenzolar-S-methyl 5.8 4.7 77 4.4 Spirotetramat 5.9. 55 8.7 Flusilazole 5.9.4 9 0. Picoxystrobin 5.9 08.5 0 8.7 Prothioconazole 5.40 09.5 54. Penconazole 5.40 09. 9 6.4 Dimoxystrobin 5.4 09.5 0 8.4 Epoxiconazole 5.4.7 86 6.9 Diniconazole 5.4 06.7 05 5. Mefenacet 5.44 4.8 89 9.9 Bitertanol 5.44 09.7 9 6.9 Metconazole 5.45 09.0 76 6.7 Butafenacil 5.46 4.9 4.5 Etaconazole isomer 5.47 5.6 89 8.8 Dimethomorph isomer 5.48 8.4 88 6.7 Fluquinconazole 5.48 6.8 90 4.6 Fenbuconazole 5.48.7 94. Dimethomorph isomer 5.49 8.6 89 6. Kresoxim-methyl 5.49 09.8 78 7. Fluoxastrobin 5.50 4.6 7 5.8 Mandipropamid 5.5 4.0 84.7 Famoxadone 5.5.4 5 4.5 Thiobencarb 5.56 08.4 90.7 Ipconazole isomer 5.56 07.5 96.4. Ipconazole isomer 5.56 07.5 04 4.8 Amitraz 5.59.6 9 9.9 Benalaxyl 5.59. 98.4 Pencycuron (Monceren) 5.60 09.8 90 6.7 Bromucanozole isomer 5.6 9.6 99. Clofentezine 5.6 08.9 9 4.4 Propiconazole isomer 5.64.0 9 8.9 Propiconazole isomer 5.64.0 86 8. Benzoximate 5.65 09.5 99 0.9 Pyraclostrobin 5.68.4 96 0.8 Prochloraz 5.69 6.8 96 8.0 Tebufenpyrad 5.69 07.6 7.5 Bromucanozole isomer 5.70. 89 5.4 Buprofezin 5.70 0. 4 4.6 Difenoconazole isomer 5.78.8 0.5 Piperonyl butoxide 5.8 08.0.7 Pyriproxyfen 5.8 07.4.5 Furathiocarb 5.85 0.4 6.4 Quinoxyfen 5.97 0. 95 4.8 Hexythiazox 5.98 0.5 0.7 Rotenone 6.00. 00 9.7 Fast analyses for sophisticated separations LC/MS analysis of more than 50 pesticides in less than 6.5 minutes on. Standard deviation [%] Continued on page 8 7
Continued from page 7 Relative retention times in comparison to NUCLEOSHELL Bluebird RP 8 for selected analytes 80 60 40 0 Relative retention time [%] 00 80 60 40 0 0 4 5 6 7 8 9 0 4 5 6 7 8 9 0 4 5 6 7 8 9 0 Aminocarb 9 Mexacarbate 7 Cymoxanil 5 Fenpropimorph Propamocarb 0 Flonicamid 8 Butocarboxim 6 Methoprotryne Formetanate HCI Methomyl 9 Simetryn 7 Oxadixyl 4 Pymetrozine Fuberidazole 0 Secbumeton 8 Thiacloprid 5 Aldicarb sulfoxide Ethirimol Acetamiprid 9 Bromucanozole isomer 6 Carbendazim 4 Imidacloprid Imazalil 0 Rotenone 7 Aldicarb sulfone 5 Primicarb Spiroxamine isomer 8 Nitenpyram 6 Prometon 4 Spiroxamine isomer Alternative selectivity and high hydrophobicity Highly increased retention (alternative selectivity) for certain aryl compounds compared to a core-shell octadecylsilyl modifi cation in methanol. The comparison with NUCLEOSHELL Bluebird RP 8 also proves the high hydrophobicity compared to other aryl phases. 8
Phthalates MN Appl. No. 880 EC 00/,.7 μm EC 00/ NUCLEOSHELL Phenyl-Hexyl,.7 μm EC 00/ NUCLEOSHELL PFP,.7 μm MN REF: 7664.0, 7674.0, 7654.0 Temperature: 0 C A) water B) 0. % water in acetonitrile hold 50 % B for.5 min, in 6.0 min to 95 % B, hold 95 % B for.5 min, in.0 min to 50 % B, hold 50 % B for 4.5 min.0 ml/min UV, 8 nm 5 μl 0.0 ng/ml for each analyte in water acetonitrile (:, v/v) Chromatograms Retention times Analyte Biphenyl RT [min] Phenyl-Hexyl RT [min] PFP RT [min] Dimethyl phthalate 0.96 0.94 0.86 Diethyl phthalate.50.49.0 Dipropyl phthalate.87.80.89 4 Dibutyl phthalate 4.09 4..99 5 Benzyl butyl phthalate 4.4 4.9.07 6 Dicyclohexyl phthalate 5.9 5.6.78 7 Diheptyl phthalate 6.80 6.87 5.6 8 Dioctyl phthalate 7.44 7.5 5.80 Superior aromatic selectivity is able to baseline separate the critical pair dibuthyl phthalate / benzyl butyl phthalate whereas other aryl phases cannot achieve this. 4 5 6 5 7 4 6 8 7 4 5 8 6 7 8 NUCLEOSHELL PFP NUCLEOSHELL Phenyl-Hexyl 0 4 5 6 7 min 9
Estrogens MN Appl. No. 8850 EC 50/,.7 μm MN REF: REF 766.0 A) 0.0 mm ammonium fl uoride in water B) acetonitrile from 0 % to 50 % B in 5 min, in.0 min to 99 % B, hold 99 % B for.5 min, in 0.5 min to 0 % B, hold 0 % B for.0 min Temperature: 0 C 0.0 ml/min MS, MRM 0 μl 0.0 ng/ml for each analyte in eluent A methanol (9:, v/v) MRM transitions Analyte RT [min] [M-H] Q (Quantifier) Q (Qualifier) Estradiol 0.0 7. 8. 45. Estrone. 95. 45. 4. Ethynylestradiol.7 69. 45. 67. Chromatogram Intensity [cps] 6.0e5 5.0e5 4.0e5.0e5.0e5.0e5 0.0 9.0 9.5 0.0 0.5.0.5.0.5 min DNPH aldehydes MN Appl. No. 8840 EC 50/,.7 μm MN REF: REF 766.0 Temperature: 40 C A) water B) acetonitrile in 5.0 min from 0 % to 7 % B, hold 7 % B for.0 min, in.0 min to 0 % B, hold 0 % B for 5.0 min.0 ml/min UV, 60 nm 0 μl 0.5 µg/ml for each analyte in water acetonitrile (95:5, v/v) Retention times Analyte RT [min] Formaldehyde.58 Acetaldehyde.86 Acetone.09 Isobutyraldehyde + p-tolualdehyde.6 Hexanal.55 Butanal + o- / m-tolualdehyde.64 Pentanal.7,5-Dimethylbenzaldehyde.77 Octanal 4.05 Nonanal 4.9 Decanal 4.6 For further analytes the following retention times have been determined (not presented in the chromatogram): Analyte RT [min] Propanal.4 Acrolein. Isovaleraldehyde.56 Benzaldehyde.59 Crotonaldehyde.7 Cyclohexanon.77 Chromatogram Absorbance [mau].5.5 0.5 0.5.5 4 4.5 min 0
Algal toxins in mussels MN Appl. No. 8860 EC 50/,.7 μm EC 50/ NUCLEODUR π, 5 μm MN REF: 7666.0, 76065.0 Temperature: 40 C A) 50 mm formic acid B) methanol hold 79 % B for 4.0 min, in 0. min to 8 % B, in 0.9 min to 86 % B, in 0. min to 98 % B, hold 98 % B for.9 min, in 0. min to 79 % B 0.0 ml/min MS, MRM 0 μl 0.0 ng/ml for each analyte MRM transitions Analyte RT [min] [M+H] + Q (Quantifier) Q (Qualifier) Okadaic acid 9.5 87.5 809.4 7.4 Dinophysistoxin- 0. 87.5 809.4 7.4 Dinophysistoxin-.7 84.5 8.4 77.4 Pectenotoxin- 7. 88. 87.4 59. Chromatograms Intensity [cps] 8.0e4 6.0e4 4.0e4 0 5 0 min.0e4 5 0 5 0 min We thank TeLA GmbH for the cooperation and for the method development of this application. Advantage of core-shell vs fully porous particles Improved peak shape and better baseline separation with in comparison to NUCLEODUR π².
Ordering information Length 50 mm 00 mm 50 mm,.7 µm EC columns (pack of ) mm ID 766.0 7664.0 7666.0 mm ID 766.0 7664.0 7666.0 4 mm ID 766.40 7664.40 7666.40 4.6 mm ID 766.46 7664.46 7666.46 Extend your column lifetime with our selection of guard columns For EC column with ID of REF guard column Required guard column holder (Column protection system) mm EC 4/ (pack of ) 7668.0 78966 / 4 / 4.6 mm EC 4/ (pack of ) 7668.0 78966 Registered trademarks NUCLEOSHELL Kinetex Raptor HALO MACHEREY-NAGEL GmbH & Co. KG (Germany) Phenomenex (USA) Restek (USA) Advanced Materials Technology (USA) MACHEREY-NAGEL shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing, performance, or use of this material. Information, descriptions, and specifications in this publication are subject to change without notice. Your local distributor rgb (S. ), fotomek (S. 4), Sven Hastedt (S. 5), Inga Nielsen (S. 8), ilolab (S. ) fotolia.com KATEN0074 Broschüre en / / 0 / 0.08 DD Printed in Germany MACHEREY-NAGEL GmbH & Co. KG Neumann-Neander-Str. 6 8 555 Düren Germany DE / International: Tel.: +49 4 969-0 Fax: +49 4 969-99 E-mail: info@mn-net.com CH: Tel.: +4 6 88 55 00 Fax: +4 6 88 55 05 E-mail: sales-ch@mn-net.com FR: Tel.: + 88 68 68 Fax: + 88 5 76 88 E-mail: sales-fr@mn-net.com US: Tel.: + 484 8 0984 Fax: + 484 8 7 E-Mail: sales-us@mn-net.com