WO2000039562A1 - Analyse de vitamines par spectroscopie proche infrarouge - Google Patents

Analyse de vitamines par spectroscopie proche infrarouge Download PDF

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Publication number
WO2000039562A1
WO2000039562A1 PCT/EP1999/010502 EP9910502W WO0039562A1 WO 2000039562 A1 WO2000039562 A1 WO 2000039562A1 EP 9910502 W EP9910502 W EP 9910502W WO 0039562 A1 WO0039562 A1 WO 0039562A1
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WO
WIPO (PCT)
Prior art keywords
vitamin
vitamins
near infrared
composition
spectrum
Prior art date
Application number
PCT/EP1999/010502
Other languages
English (en)
Inventor
Jean-Christophe Bodin
Laurent Dussert
Thomas D'alfonso
Original Assignee
Aventis Animal Nutrition S.A.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Aventis Animal Nutrition S.A. filed Critical Aventis Animal Nutrition S.A.
Priority to AU21047/00A priority Critical patent/AU2104700A/en
Publication of WO2000039562A1 publication Critical patent/WO2000039562A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water

Definitions

  • the present invention relates to a novel process for the qualitative and quantitative analytical determination of a vitamin or a mixture of vitamins and in particular to a process for the qualitative and quantitative determination of vitamins using near infrared spectroscopy .
  • premixes intended for animal feed can be in the form of liquid mixtures or in a solid form.
  • the vitamin premix when it is in the liquid form, it often contains diluents, surfactant and stabilisers.
  • the premix When the premix is in solid form, the composition often contains a support for example of mineral or plant origin, as well as food additives such as amino acids and/or vitamins. After preparation of the premix, it is preferable to check the composition and/or homogeneity of these mixtures by means of a rapid and non-destructive analytical technique.
  • Zootech (1993) 42, 251-270 who established calibration curves for the following analyses: solids content, ash content, total proteins, water-soluble carbohydrates, celluloses, cell wall constituents, total fibres, acidic and neutral detergent fibres, lignin, enzymatic solubilities determined by the Aufrere, Limagrain and Lila methods.
  • This combination of "in vitro" analyses has made it possible to carry out near-infrared analyses and, with the aid of a statistical analysis, to establish correlation curves which henceforth allow a direct near-infrared spectroscopy determination of the digestibility value "in vivo".
  • the present application provides a method for the determination of the presence of one or more vitamins in a composition containing the vitamin characterised in that the presence is determined by near infrared spectroscopy.
  • the method comprises
  • step (e) comparing the spectrum obtained in step (d)with the spectra of the data base to identify the vitamin and determining the concentration of vitamin from the collaboration plot.
  • the presence is meant the identity of the vitamin and the amount of the vitamin.
  • near infrared is meant the region of the spectrum ranging from 700 to 2500 nm.
  • the present invention relates to a novel method for the direct determination of the presence of one or more vitamins in a composition containing at least one vitamin.
  • the method relates in general to the direct determination of the emission or transmission spectrum of the composition containing the vitamin in the near-infrared range and then in applying chemometric algorithms to the spectrum in order to determine the vitamin concentration.
  • the present method is generally not affected by the presence of the matrix in the composition even if the composition is a complex mixture, such as the various liquid supports containing the mixture of vitamins or the various solid supports constituting the basic vitamin premix to which the vitamins are added.
  • the present invention is a non- invasive technique which avoids the need to extract the vitamins, which always carries uncertainty regarding the quality of the extraction, and avoids the need to undertake subsequent reactions which consume time and thus money.
  • the subject of the present invention is the qualitative and/or quantitative determination of the presence of vitamins which may be in a liquid or solid vitamin complex; a mixture of vitamins and/or in a vitamin premix which, in this case also, may be liquid or solid, this complex or mixture being intended to be incorporated into whole foods for man or feeds for rearing animals, by near-infrared spectroscopy.
  • the method of the present invention is used to determine the presence of at least one vitamin in a vitamin-containing composition.
  • the method is particularly suitable for the determination of vitamin E or tocopherol in esterified form (acetate) , vitamin B5 or calcium D-pantothenate, vitamin D3 or cholecalciferol, vitamin PP or niacin in the acid or amide form, vitamin BI or thiamine mononitrate, vitamin B2 or riboflavin, vitamin B6 or pyridoxine hydrochloride, vitamin H or biotin, vitamin B12 or cyanocobalamin, vitamin C or ascorbic acid, vitamin A or retinol in esterified form (acetate, palmitate or propionate) , vitamin K3 or menadione and vitamin B9 or folic acid.
  • the method of determination may be applied to a composition containing an individual vitamin or to a composition comprising a mixture of vitamins.
  • the composition may comprise a liquid and/or solid support which may be liquid or solid.
  • the support used in the solid premixes can be chosen from supports of mineral or plant origin.
  • the mineral supports which may be mentioned are calcium carbonate, dicalcium phosphate and sodium chloride.
  • the plant supports which may be mentioned in a non-limiting manner, are wheat or rice bran, middlings, soya cake and corn husks.
  • These premixes can also contain microelements such as iron, cobalt, copper, manganese, molybdenum, selenium and zinc salts with various hydration contents.
  • the method of the present invention comprises the creation of a data base. This procedure involves the accumulation of chemical analytical data for a number of known proteins and/or protein mixtures.
  • the method for chemical determination of the vitamin consists in carrying out a conventional chemical analysis of a population of representative samples of the variation range in terms of composition which may be expected in practice. For reasons of statistical reliability, a minimum of 80, preferably at least 120 samples may be used to start the construction of such a type of mathematical model .
  • the corresponding near infrared spectrum for each sample is recorded by means of a spectrophotometer working in the near-infrared range (i.e. between 700 and 2500 nm) .
  • the measurement taken is in the form of a spectrum which in fact bears information regarding the physicochemical composition of the sample.
  • the two sets of results are recorded and stored, thus establishing a database of the results obtained by chemical analysis and the absorbance values measured by near infrared spectroscopy.
  • a calibration plot is then prepared, by mathematical processing of the infra red spectroscopy data, using appropriate computer software.
  • the mathematical processing provides a linear regression which makes it possible to establish a prediction curve.
  • the management of these operations can be carried out by means of any suitable commercially available software system.
  • the accuracy of the relationship between the near infrared analysis and the chemical analysis may be verified by recording the spectrum of samples of vitamin of known concentration using samples which have not been used to establish the calibration curve.
  • the results obtained after the mathematical treatment may be compared with the calibration curve.
  • the next step of the method of the present invention comprises recording the infra red spectrum of the vitamin-containing composition.
  • the spectrum, thus obtained is compared with the spectra stored in the date base.
  • the spectrum, thus obtained is subjected to the same mathematical treatment as the calibration samples to provide a number. As proven from the calibration plot, this number corresponds to the concentration of vitamin.
  • the quality control method may be carried out by the vitamin manufacturer or the breeder.
  • Step 1 Construction of a calibration population
  • a calibration population of 120 samples of vitamin-containing compositions was prepared which involved the preparation of data base of chemical analysis results and near infrared spectra.
  • the chemical analysis of the vitamin- containing composition was carried out for each sample as per the standard routine analysis for the particular vitamin to qualitatively and quantitatively identify either the vitamin and/or the vitamins in the composition
  • the samples were also analysed using near infra red spectroscopy wherein the spectrum of each sample was obtained in the region of 700 to 2500nm.
  • the spectrum of each sample was recorded using a grating spectrophotometer of NIRS 6500 type (sold by FOSS Int.) operating in "reflectance" mode.
  • NIRS 6500 type sold by FOSS Int.
  • a particular specificity of the instrument was that it worked over the entire near-infrared range rather than over a number of specific wavelengths, as is the case for certain more conventional machines .
  • the sample was packaged in a rectangular transportation cell composed of three opaque faces and a face fitted with a quartz crystal. After positioning the cell in the spectrophotometer, the light reflected by the sample, which bears information regarding the chemical composition of this sample, was recorded in the form of a spectrum. Each type of product, and consequently each sample, has a different spectrum.
  • the results from the chemical and spectroscopic analyses were stored in a data base and identified as the calibration file. The calibration file thus contained a combination of numerical and spectral data.
  • the entire calibration file constructed was subjected to a statistical calculation using suitable software (NIRS 2, version 3.00 distributed by Infrasolt International I.S.I.) which made it possible to detect the presence of non-standard spectra which have excessively large Mahalanobis distances (statistical distance H) compared with the average spectrum of the population (centre of gravity) . Once detected, these samples were eliminated in order to obtain homogeneous population.
  • suitable software NIRS 2, version 3.00 distributed by Infrasolt International I.S.I.
  • the calibration file containing all the samples was then subjected to a statistical analysis, of which three different types exist: "Modified Partial Least Square” (MPLS), Partial Least Square (PLS), which is a general form of regression by main components, or “step up", which corresponds to a simpler linear regression.
  • MPLS Modified Partial Least Square
  • PLS Partial Least Square
  • step up which corresponds to a simpler linear regression.
  • Figures 1/6 to 4/6 show, respectively, the calibration curves for vitamins A, E, B5 and PP in vitamin mixtures
  • Figures 5/6 to 6/6 represent calibration curves for vitamins E and A established on food premixes on an organic support containing various mineral salts.
  • the near infrared spectrum of the unknown sample was recorded and entered into the data base to find a corresponding spectrum.
  • the vitamin was therefore identified qualitatively.
  • the spectrum was subjected to the same statistical calculation as the database samples to obtain a figure which corresponds to the concentration of the vitamin as verified by the calibration.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

La présente invention concerne une méthode permettant de déterminer la présence d'une ou de plusieurs vitamines dans une composition renfermant ladite vitamine par spectrophotométrie proche infrarouge.
PCT/EP1999/010502 1998-12-23 1999-12-22 Analyse de vitamines par spectroscopie proche infrarouge WO2000039562A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU21047/00A AU2104700A (en) 1998-12-23 1999-12-22 Near infrared spectroscopic analysis of vitamins

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9816362 1998-12-23
FR98/16362 1998-12-23

Publications (1)

Publication Number Publication Date
WO2000039562A1 true WO2000039562A1 (fr) 2000-07-06

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Family Applications (1)

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PCT/EP1999/010502 WO2000039562A1 (fr) 1998-12-23 1999-12-22 Analyse de vitamines par spectroscopie proche infrarouge

Country Status (2)

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AU (1) AU2104700A (fr)
WO (1) WO2000039562A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102058682A (zh) * 2009-11-17 2011-05-18 天津天士力现代中药资源有限公司 一种白芍提取液中的芍药苷含量的nir在线检测方法
CN102636449A (zh) * 2011-06-15 2012-08-15 江西本草天工科技有限责任公司 一种近红外光谱测定白芍提取过程中芍药苷含量的方法
CN111896604A (zh) * 2020-06-05 2020-11-06 中芯维康医疗科技(重庆)有限责任公司 一种维生素检测仪质控品组合物及其应用

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5506117A (en) * 1989-10-18 1996-04-09 Cytokinetics, Inc. Biochemical process for growing living cells by measuring the amount of nutrient added to the reaction medium
WO1997021091A1 (fr) * 1995-12-01 1997-06-12 Commonwealth Scientific And Industrial Research Organisation Procede d'evaluation de la qualite d'aliments pour animaux
DE29809591U1 (de) * 1997-09-04 1998-09-24 Basf Ag, 67063 Ludwigshafen Vorrichtung zur Identifizierung von Wirkstoffen

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5506117A (en) * 1989-10-18 1996-04-09 Cytokinetics, Inc. Biochemical process for growing living cells by measuring the amount of nutrient added to the reaction medium
WO1997021091A1 (fr) * 1995-12-01 1997-06-12 Commonwealth Scientific And Industrial Research Organisation Procede d'evaluation de la qualite d'aliments pour animaux
DE29809591U1 (de) * 1997-09-04 1998-09-24 Basf Ag, 67063 Ludwigshafen Vorrichtung zur Identifizierung von Wirkstoffen

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
HANCEWITCZ T. M. AND PETTY C.: "Quantitative analysis of vitamin A using Fourier transform Raman spectroscopy.", SPECTROCHIMICA ACTA PART A, vol. 51, 4 May 1995 (1995-05-04), pages 2193 - 2198, XP002115781 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102058682A (zh) * 2009-11-17 2011-05-18 天津天士力现代中药资源有限公司 一种白芍提取液中的芍药苷含量的nir在线检测方法
CN102636449A (zh) * 2011-06-15 2012-08-15 江西本草天工科技有限责任公司 一种近红外光谱测定白芍提取过程中芍药苷含量的方法
CN111896604A (zh) * 2020-06-05 2020-11-06 中芯维康医疗科技(重庆)有限责任公司 一种维生素检测仪质控品组合物及其应用

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Publication number Publication date
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