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HPLC-MS detection method of xanthophylls cis-trans-isomers in xanthophylls products

A technology of cis-trans isomerization and detection method, which is applied in the field of liquid chromatography analysis, can solve the problems of poor separation effect of lutein isomers, relatively expensive prices of acetonitrile and methyl tert-butyl ether, and achieve separation Good effect, extended retention time, high sensitivity effect

Inactive Publication Date: 2013-04-03
NORTHEAST FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Zhang Yan et al reported a YMC-C 30 The method for separating lutein and its isomers by chromatographic column uses mobile phases of methyl tert-butyl ether, methanol and acetonitrile, the separation effect of lutein isomers is not very good, and acetonitrile and methyl tert-butyl ether more expensive

Method used

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  • HPLC-MS detection method of xanthophylls cis-trans-isomers in xanthophylls products
  • HPLC-MS detection method of xanthophylls cis-trans-isomers in xanthophylls products
  • HPLC-MS detection method of xanthophylls cis-trans-isomers in xanthophylls products

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Weigh 0.01 g of the content of lutein soft capsules into a conical flask, add 30 mL of extractant (hexane-acetone-ethanol-toluene), plug the stopper and fully rotate and shake. Use a pipette to add 2mL of 40% KOH methanol solution to the Erlenmeyer flask, rotate and shake for 1min, seal overnight (12h), transfer the sample solution to a separatory funnel, wash with 10% sodium sulfate, and wash several times to remove the lye . Take the supernatant, concentrate to dryness under reduced pressure, dilute to 10 mL with methanol, and filter the sample liquid through a 0.45 μm microporous membrane for later use. HPLC-MS detection of lutein isomers in soft capsules, in which the content of all-trans lutein is 3.68mg / g, the content of 9-cis-lutein is 0.056mg / g, and the content of 9'-cis-lutein 0.06mg / g, 13-cis-lutein content 0.12mg / g and 13'-cis-lutein content 0.128mg / g.

[0049] C 30 -HPLC analysis conditions: chromatographic column is YMC Carotenoid C 30 (4.6mm×250mm, 5μm...

Embodiment 2

[0051] Powder the lutein tablet, weigh 0.01g of the powder into a conical flask, add 30mL extractant (hexane-acetone-ethanol-toluene), plug the stopper and fully rotate and shake. Use a pipette to add 2mL of 40% KOH methanol solution to the Erlenmeyer flask, rotate and shake for 1min, seal overnight (12h), transfer the sample solution to a separatory funnel, wash with 10% sodium sulfate, and wash several times to remove the lye . Take the supernatant, concentrate to dryness under reduced pressure, dilute to 10 mL with methanol, and filter the sample liquid through a 0.45 μm microporous membrane for later use. HPLC-MS detection of lutein isomers in the tablet, in which the content of all-trans lutein is 13.76mg / g, the content of 9-cis-lutein is 0.35mg / g, and the content of 9'-cis-lutein 0.37mg / g, 13-cis-lutein content 0.77mg / g and 13'-cis-lutein content 0.82mg / g.

[0052] C 30 -HPLC analysis conditions: chromatographic column is YMC Carotenoid C 30 (4.6mm×250mm, 5μm), mobil...

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Abstract

The invention belongs to the field of analysis technology, and relates to an HPLC-MS detection method of xanthophylls cis-trans-isomers in xanthophylls products. The method is characterized by performing a light iodine isomerization reaction for the all-trans xanthophylls to obtain the cis-isomeride of the xanthophylls; using a YMC Carotenoid C30 chromatographic column to substantially separate the xanthophylls isomer, wherein a mobile phase is methanol / water = 98 / 2, a time is 70 minutes, a flow velocity rate is 1.0 mL / min, a DAD detector is used, a column temperature is 25 DEG C, an injection volume is 20 [mu]l and a detection wavelength is 450 nm; and using a positive ion mass spectrometry (APCI / MS), wherein a flow rate of the components from the chromatographic column into the mass spectrometer is 10 [mu]L / min, a scanning range m / z is 200 to 800, a capillary temperature is 150 DEG C, a vaporization temperature is 450 DEG C, a capillary voltage is 10 V, and a flow rate of dry gases is 8 mL / min. According to information of the mass spectrum and the spectrum, the xanthophylls isomers are respectively determined as all trans, 9-cis, 9'-cis, 13-cis and 13'-cis xanthophylls. The analysis method is rapid and effective, good in reproducibility and high in recovery rate, and can quantitatively analyze content of the xanthophylls cis-trans-isomers in the xanthophylls products.

Description

technical field [0001] The invention relates to an HPLC-MS detection method of lutein cis-trans isomers in lutein products, and belongs to the technical field of liquid chromatography analysis. Background technique [0002] Lutein, an oxygen-containing carotenoid, is widely found in vegetables, flowers, fruits and some algae, especially in marigold flowers. Because lutein can absorb a large amount of blue light close to ultraviolet light, it can filter blue light that damages photoreceptors and retinal pigment epithelium. Timely supplementation of lutein can prevent vision loss and blindness caused by age-related macular degeneration (AMD). In addition, lutein also has physiological functions such as anti-oxidation, anti-cancer, anti-mutagenesis, and delaying arteriosclerosis. It is a functional pigment with natural nutrition and health. [0003] At present, commercial lutein is mainly extracted and separated from marigold oleoresin. However, lutein is insoluble in water a...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 李大婧黄占华王闯李德海
Owner NORTHEAST FORESTRY UNIVERSITY
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