IPC분류정보
국가/구분 |
United States(US) Patent
등록
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국제특허분류(IPC7판) |
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출원번호 |
UP-0242210
(2005-10-03)
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등록번호 |
US-7566401
(2009-08-05)
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발명자
/ 주소 |
- Kelm, Mark A.
- Johnson, Christopher J.
- Robbins, Rebecca J.
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인용정보 |
피인용 횟수 :
2 인용 특허 :
3 |
초록
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An improved process for separating and isolating individual polar protic monomer(s) and/or oligomer(s) on the basis of degree of polymerization. A liquid sample containing polar protic monomer(s) and/or oligomer(s) is introduced into a liquid chromatography (LC) column packed with a polar bonded st
An improved process for separating and isolating individual polar protic monomer(s) and/or oligomer(s) on the basis of degree of polymerization. A liquid sample containing polar protic monomer(s) and/or oligomer(s) is introduced into a liquid chromatography (LC) column packed with a polar bonded stationary chromatographic phase. The individual polar protic monomer(s) and/or oligomer(s) are separated via a binary mobile phase elution. One or more individual fractions containing the monomer(s) and/or oligomer(s) are eluted. The polar protic monomer(s) and/or oligomer(s) may be proanthocyanidins, hydrolyzable tannins, oligosaccharides, oligonucleotides, peptides, acrylamides, polysorbates, polyketides, poloxamers, polyethylene glycols, polyoxyethylene alcohols or polyvinyl alcohols. The binary mobile phase comprises an A phase consisting essentially of a polar aprotic solvent and a B phase consisting essentially of a polar protic solvent. A process for separating and isolating xanthine(s) (e.g., caffeine and theobromine) from polar protic monomer(s) and/or oligomer(s). A liquid sample containing xanthine(s) and polar protic monomer(s) and/or oligomer(s) is introduced into an LC column packed with a polar bonded stationary chromatographic phase. The xanthines are separated via an isocratic mobile phase elution, and one or more individual fractions containing the xanthines are eluted.
대표청구항
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What is claimed is: 1. A normal phase high performance liquid chromatographic process for separating, eluting, and isolating xanthine(s) and polar protic monomer(s) from polar protic oligomer(s) comprises the steps of: (a) introducing a liquid sample containing the xanthine(s), the polar protic mon
What is claimed is: 1. A normal phase high performance liquid chromatographic process for separating, eluting, and isolating xanthine(s) and polar protic monomer(s) from polar protic oligomer(s) comprises the steps of: (a) introducing a liquid sample containing the xanthine(s), the polar protic monomer(s), and the polar protic oligomer(s) into a liquid chromatography column packed with a polar bonded stationary phase selected from the group consisting of a diol phase, a glycerol phase, an amino phase, a cyano phase, a trimethylsilyl phase, a dimethylsilyl phase, a halogenated phase, and a nitro phase; (b) passing an isocratic mobile phase consisting essentially of a polar aprotic solvent through the column to elute the xanthine(s) and the polar protic monomer(s); (c) isolating one or more individual fractions containing the xanthine(s) and the polar protic monomer(s); and (d) optionally recovering the isolated xanthine(s) and/or the isolated polar protic monomer(s). 2. A normal phase high performance liquid chromatographic process for separating, eluting, and isolating xanthine(s), individual polar protic monomer(s), and individual polar protic oligomer(s) comprises the steps of: (a) introducing a liquid sample containing the xanthine(s) the polar protic monomer(s), and the polar protic oligomer(s) into a liquid chromatography column packed with a polar bonded stationary phase selected from the group consisting of a diol phase, a glycerol phase, an amino phase, a cyano phase, a trimethylsilyl phase, a dimethyisilyl phase, a halogenated phase, and a nitro phase; (b) passing an isocratic mobile phase consisting essentially of a polar aprotic solvent through the column to elute the xanthine(s) and the polar protic monomer(s); (c) isolating one or more individual fractions containing the xanthine(s) and the polar protic monomer(s); (d) passing a binary mobile phase comprising an A phase consisting essentially of a polar aprotic solvent and a B phase consisting essentially of a polar protic solvent through the column to elute the individual polar protic oligomer(s) on the basis of degree of polymerization; (e) isolating one or more individual fractions containing the polar protic oligomer(s); and (f) optionally recovering the isolated xanthine(s), the isolated polar protic monomer(s), and/or the isolated polar protic oligomer(s). 3. The process of claim 1, or 2, wherein the polar protic oligomers are proanthocyanidin oligomers selected from the group consisting of proapigeninidins, proluteolinidins, protricetinidins, propelargonidins, procyanidins, prodelphinidins, proguibourtinidins, profisetinidins, prorobinetinidins, proteracacinidins, and promelacacinidins. 4. The process of claim 1, or 2, wherein the polar protic monomer(s) are epicatechin and/or catechin and the polar protic oligomer(s) are procyanidins. 5. The process of claim 1, or 2, wherein the liquid sample is a polar, defatted cocoa extract. 6. The process of claim 1, or 2, wherein the stationary phase is the diol phase or the glycerol phase. 7. The process of claim 1, or 2, wherein the stationary phase has a particle size from about 3 μm to about 10 μm. 8. The process of claim 1, or 2, wherein the polar aprotic solvent is acetonitrile, acetone, cyclohexanone, methyl ethyl ketone, methyl tert-butyl ether, diethyl ether, dimethyl ether, methyl acetate, ethyl acetate, or nitromethane. 9. The process of claim 2, wherein the A phase and the B phase are aqueous phases. 10. The process of claim 2, wherein the proportion of the polar aprotic solvent in the A phase is up to 100% by volume and the proportion of the polar protic solvent in the B phase is up to 100% by volume. 11. The process of claim 10, wherein the proportion of the polar aprotic solvent in the A phase is greater than 50% by volume; wherein the proportion of the polar protic solvent in the B phase is greater than 50% by volume; and wherein the remainder of the A phase and the B phase is an mineral acid, or organic acid, and/or water. 12. The process of claim 11, wherein the proportion of the polar aprotic solvent in the A phase is greater than 90% by volume; wherein the proportion of the polar protic solvent in the B phase is greater than 90% by volume; and wherein the organic acid is acetic acid. 13. The process of claim 12, wherein the A phase consists essentially of a mixture of about 98% acetonitrile and about 2% acetic acid (v/v) or a mixture of about 99% aectonitrile and 1% acetic acid (v/v) and wherein the B phase consists essentially of a mixture of about 95% methanol, about 3% water, and about 2% acetic acid (v/v/v) or a mixture of about 95% methanol, about 4% water, and about 1% acetic acid (v/v/v). 14. The process of claim 1 or 2, wherein the xanthine(s) are caffeine and/or theobromine. 15. The process of claim 1 or 2, wherein the isocratic mobile phase is an aqueous phase. 16. The process of claim 1 or 2, where wherein the proportion of the polar aprotic solvent in the isocratic mobile phase is at least 90% by volume. 17. The process of claim 16, wherein the polar aprotic solvent in the isocratic mobile phase is acetonitrile. 18. The process of claim 17, wherein the isocratic mobile phase consists essentially of about 99% acetonitrile by volume. 19. The process of claim 2, wherein the polar protic solvent is methanol, ethanol, n-propanol, isopropanol, n-butanol, or isobutanol.
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