Determination of Vitamin K in Milk and Infant Formulas by Liquid Chromatography: Collaborative Study

Harvey E. Indyk; David C. Woollard; Millie Barber; Carrie Berge; Sarah Booth; Malcolm Burn; Adriano Cecco; Scott Christiansen; Kathy Cook; Ursula Coors; Francesca Dapra; Kenneth Davidson; Marion P. De Roode; Natalie Dumais; Michael Edwards; Chris Ellis; Ibrahim Elmadfa; Giuliana Fedrigo; Bertram Fong; Pamela Gilliland; Susan Hannaford; Peter Hofmann; Peter Horstmann; Marija Jagodic; Maurice Kerr; Kaname Kodaka; Terhi Koivu-Tikkanen; Erik Konings; Jim Kyval; Bernard Lacheron; Paul Lawrence; Emile Ledoyen; Pamela Manzi; Hisashi Matsuda; Adriana McCamley; Donald Myers; Janet Nelson; Rachel Noble; Lisa Oehrl; Gianfranco Panfili; Richard Pelletier; Vieno Piironen; Laura Pizzoferrato; Sal Regala; Koichi Saito; Karen Schimpf; Willy Schuep; Leon Schurgers; Henry Simons; Enrico Tagliaferri; Henk Thijssen; Christian Tremblay; Marie Jose Trisconi; Cees Vermeer; Wijnand Verschoor; Pat Vyas; Karl Heinz Wagner; Gerald Woollard

doi:10.1093/jaoac/83.1.121

Determination of Vitamin K in Milk and Infant Formulas by Liquid Chromatography: Collaborative Study

Harvey E. Indyk, David C. Woollard, Millie Barber, Carrie Berge, Sarah Booth, Malcolm Burn, Adriano Cecco, Scott Christiansen, Kathy Cook, Ursula Coors, Francesca Dapra, Kenneth Davidson, Marion P. De Roode, Natalie Dumais, Michael Edwards, Chris Ellis, Ibrahim Elmadfa, Giuliana Fedrigo, Bertram Fong, Pamela GillilandSusan Hannaford, Peter Hofmann, Peter Horstmann, Marija Jagodic, Maurice Kerr, Kaname Kodaka, Terhi Koivu-Tikkanen, Erik Konings, Jim Kyval, Bernard Lacheron, Paul Lawrence, Emile Ledoyen, Pamela Manzi, Hisashi Matsuda, Adriana McCamley, Donald Myers, Janet Nelson, Rachel Noble, Lisa Oehrl, Gianfranco Panfili, Richard Pelletier, Vieno Piironen, Laura Pizzoferrato, Sal Regala, Koichi Saito, Karen Schimpf, Willy Schuep, Leon Schurgers, Henry Simons, Enrico Tagliaferri, Henk Thijssen, Christian Tremblay, Marie Jose Trisconi, Cees Vermeer, Wijnand Verschoor, Pat Vyas, Karl Heinz Wagner, Gerald Woollard

Publications: Contribution to journal › Article › Peer Reviewed

Abstract

A simple procedure for determination of vitamin Ki was developed for routine compliance monitoring of supplemented infant formula and measurement of endogenous levels in milk and milk powders. Samples are digested with lipase and extracted into hexane; an aliquot is evaporated, reconstituted in methanol, and analyzed by reversed-phase LC. Post-column zinc reduction of phylloquinone facilitates detection by fluorescence. The procedure was subjected to an AOAC collaborative study involving 8 materials, each in blind duplicate, across the range of 5-120 μg/100 g solids and including NIST 1846 reference material. Thirty-three laboratories returned valid data which were then statistically analyzed for outliers and precision parameters. Mean RSD_R (%) was 6.53 (4.33-10.94), with a mean HORRAT value of 0.33 (0.23-0.43) and RSD_r:RSD_R ratio of 0.74. K₁ isomers (cis and trans) were aggregated with conventional C₁₈ columns, but may be selectively estimated with use of the C₃₀ column.

Original language	English
Pages (from-to)	121-130
Number of pages	10
Journal	Journal of AOAC International
Volume	83
Issue number	1
DOIs	https://doi.org/10.1093/jaoac/83.1.121
Publication status	Published - 2000

Austrian Fields of Science 2012

303009 Nutritional sciences

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10.1093/jaoac/83.1.121

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Indyk, H. E., Woollard, D. C., Barber, M., Berge, C., Booth, S., Burn, M., Cecco, A., Christiansen, S., Cook, K., Coors, U., Dapra, F., Davidson, K., De Roode, M. P., Dumais, N., Edwards, M., Ellis, C., Elmadfa, I., Fedrigo, G., Fong, B., ... Woollard, G. (2000). Determination of Vitamin K in Milk and Infant Formulas by Liquid Chromatography: Collaborative Study. Journal of AOAC International, 83(1), 121-130. https://doi.org/10.1093/jaoac/83.1.121

@article{a038c38e4782493a9cb7daec820c4ea3,

title = "Determination of Vitamin K in Milk and Infant Formulas by Liquid Chromatography: Collaborative Study",

abstract = "A simple procedure for determination of vitamin Ki was developed for routine compliance monitoring of supplemented infant formula and measurement of endogenous levels in milk and milk powders. Samples are digested with lipase and extracted into hexane; an aliquot is evaporated, reconstituted in methanol, and analyzed by reversed-phase LC. Post-column zinc reduction of phylloquinone facilitates detection by fluorescence. The procedure was subjected to an AOAC collaborative study involving 8 materials, each in blind duplicate, across the range of 5-120 μg/100 g solids and including NIST 1846 reference material. Thirty-three laboratories returned valid data which were then statistically analyzed for outliers and precision parameters. Mean RSDR (%) was 6.53 (4.33-10.94), with a mean HORRAT value of 0.33 (0.23-0.43) and RSDr:RSDR ratio of 0.74. K1 isomers (cis and trans) were aggregated with conventional C18 columns, but may be selectively estimated with use of the C30 column.",

author = "Indyk, {Harvey E.} and Woollard, {David C.} and Millie Barber and Carrie Berge and Sarah Booth and Malcolm Burn and Adriano Cecco and Scott Christiansen and Kathy Cook and Ursula Coors and Francesca Dapra and Kenneth Davidson and {De Roode}, {Marion P.} and Natalie Dumais and Michael Edwards and Chris Ellis and Ibrahim Elmadfa and Giuliana Fedrigo and Bertram Fong and Pamela Gilliland and Susan Hannaford and Peter Hofmann and Peter Horstmann and Marija Jagodic and Maurice Kerr and Kaname Kodaka and Terhi Koivu-Tikkanen and Erik Konings and Jim Kyval and Bernard Lacheron and Paul Lawrence and Emile Ledoyen and Pamela Manzi and Hisashi Matsuda and Adriana McCamley and Donald Myers and Janet Nelson and Rachel Noble and Lisa Oehrl and Gianfranco Panfili and Richard Pelletier and Vieno Piironen and Laura Pizzoferrato and Sal Regala and Koichi Saito and Karen Schimpf and Willy Schuep and Leon Schurgers and Henry Simons and Enrico Tagliaferri and Henk Thijssen and Christian Tremblay and Trisconi, {Marie Jose} and Cees Vermeer and Wijnand Verschoor and Pat Vyas and Wagner, {Karl Heinz} and Gerald Woollard",

year = "2000",

doi = "10.1093/jaoac/83.1.121",

language = "English",

volume = "83",

pages = "121--130",

journal = "Journal of AOAC International",

issn = "1060-3271",

number = "1",

}

Indyk, HE, Woollard, DC, Barber, M, Berge, C, Booth, S, Burn, M, Cecco, A, Christiansen, S, Cook, K, Coors, U, Dapra, F, Davidson, K, De Roode, MP, Dumais, N, Edwards, M, Ellis, C, Elmadfa, I, Fedrigo, G, Fong, B, Gilliland, P, Hannaford, S, Hofmann, P, Horstmann, P, Jagodic, M, Kerr, M, Kodaka, K, Koivu-Tikkanen, T, Konings, E, Kyval, J, Lacheron, B, Lawrence, P, Ledoyen, E, Manzi, P, Matsuda, H, McCamley, A, Myers, D, Nelson, J, Noble, R, Oehrl, L, Panfili, G, Pelletier, R, Piironen, V, Pizzoferrato, L, Regala, S, Saito, K, Schimpf, K, Schuep, W, Schurgers, L, Simons, H, Tagliaferri, E, Thijssen, H, Tremblay, C, Trisconi, MJ, Vermeer, C, Verschoor, W, Vyas, P, Wagner, KH & Woollard, G 2000, 'Determination of Vitamin K in Milk and Infant Formulas by Liquid Chromatography: Collaborative Study', Journal of AOAC International, vol. 83, no. 1, pp. 121-130. https://doi.org/10.1093/jaoac/83.1.121

TY - JOUR

T1 - Determination of Vitamin K in Milk and Infant Formulas by Liquid Chromatography

T2 - Collaborative Study

AU - Indyk, Harvey E.

AU - Woollard, David C.

AU - Barber, Millie

AU - Berge, Carrie

AU - Booth, Sarah

AU - Burn, Malcolm

AU - Cecco, Adriano

AU - Christiansen, Scott

AU - Cook, Kathy

AU - Coors, Ursula

AU - Dapra, Francesca

AU - Davidson, Kenneth

AU - De Roode, Marion P.

AU - Dumais, Natalie

AU - Edwards, Michael

AU - Ellis, Chris

AU - Elmadfa, Ibrahim

AU - Fedrigo, Giuliana

AU - Fong, Bertram

AU - Gilliland, Pamela

AU - Hannaford, Susan

AU - Hofmann, Peter

AU - Horstmann, Peter

AU - Jagodic, Marija

AU - Kerr, Maurice

AU - Kodaka, Kaname

AU - Koivu-Tikkanen, Terhi

AU - Konings, Erik

AU - Kyval, Jim

AU - Lacheron, Bernard

AU - Lawrence, Paul

AU - Ledoyen, Emile

AU - Manzi, Pamela

AU - Matsuda, Hisashi

AU - McCamley, Adriana

AU - Myers, Donald

AU - Nelson, Janet

AU - Noble, Rachel

AU - Oehrl, Lisa

AU - Panfili, Gianfranco

AU - Pelletier, Richard

AU - Piironen, Vieno

AU - Pizzoferrato, Laura

AU - Regala, Sal

AU - Saito, Koichi

AU - Schimpf, Karen

AU - Schuep, Willy

AU - Schurgers, Leon

AU - Simons, Henry

AU - Tagliaferri, Enrico

AU - Thijssen, Henk

AU - Tremblay, Christian

AU - Trisconi, Marie Jose

AU - Vermeer, Cees

AU - Verschoor, Wijnand

AU - Vyas, Pat

AU - Wagner, Karl Heinz

AU - Woollard, Gerald

PY - 2000

Y1 - 2000

N2 - A simple procedure for determination of vitamin Ki was developed for routine compliance monitoring of supplemented infant formula and measurement of endogenous levels in milk and milk powders. Samples are digested with lipase and extracted into hexane; an aliquot is evaporated, reconstituted in methanol, and analyzed by reversed-phase LC. Post-column zinc reduction of phylloquinone facilitates detection by fluorescence. The procedure was subjected to an AOAC collaborative study involving 8 materials, each in blind duplicate, across the range of 5-120 μg/100 g solids and including NIST 1846 reference material. Thirty-three laboratories returned valid data which were then statistically analyzed for outliers and precision parameters. Mean RSDR (%) was 6.53 (4.33-10.94), with a mean HORRAT value of 0.33 (0.23-0.43) and RSDr:RSDR ratio of 0.74. K1 isomers (cis and trans) were aggregated with conventional C18 columns, but may be selectively estimated with use of the C30 column.

AB - A simple procedure for determination of vitamin Ki was developed for routine compliance monitoring of supplemented infant formula and measurement of endogenous levels in milk and milk powders. Samples are digested with lipase and extracted into hexane; an aliquot is evaporated, reconstituted in methanol, and analyzed by reversed-phase LC. Post-column zinc reduction of phylloquinone facilitates detection by fluorescence. The procedure was subjected to an AOAC collaborative study involving 8 materials, each in blind duplicate, across the range of 5-120 μg/100 g solids and including NIST 1846 reference material. Thirty-three laboratories returned valid data which were then statistically analyzed for outliers and precision parameters. Mean RSDR (%) was 6.53 (4.33-10.94), with a mean HORRAT value of 0.33 (0.23-0.43) and RSDr:RSDR ratio of 0.74. K1 isomers (cis and trans) were aggregated with conventional C18 columns, but may be selectively estimated with use of the C30 column.

UR - http://www.scopus.com/inward/record.url?scp=0033630972&partnerID=8YFLogxK

U2 - 10.1093/jaoac/83.1.121

DO - 10.1093/jaoac/83.1.121

M3 - Article

C2 - 10693013

AN - SCOPUS:0033630972

SN - 1060-3271

VL - 83

SP - 121

EP - 130

JO - Journal of AOAC International

JF - Journal of AOAC International

IS - 1

ER -

Determination of Vitamin K in Milk and Infant Formulas by Liquid Chromatography: Collaborative Study

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Austrian Fields of Science 2012

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