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Method for rapidly measuring rhodamine B by eutectic solvent extraction-liquid chromatography

A deep eutectic solvent and rapid determination technology, which is applied in the field of non-food coloring detection in food, can solve the problems of high cost, complicated process, and long time consumption, and achieve the effect of low cost, simple operation, and shortened time

Inactive Publication Date: 2017-01-04
SHENZHEN ACAD OF METROLOGY & QUALITY INSPECTION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in recent years, the illegal addition of rhodamine B in food has become more prominent after the government has stepped up its crackdown on illegal food coloring Sudan Red
At present, there is no national standard for the detection of rhodamine B in food in my country. The commonly used detection method is the entry-exit inspection and quarantine industry standard SN / T 2430-2010 promulgated in 2010, but this method needs to be used in the detection of chili oil. Gel chromatography purification system for sample pretreatment, the process is complex, costly and time-consuming

Method used

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  • Method for rapidly measuring rhodamine B by eutectic solvent extraction-liquid chromatography
  • Method for rapidly measuring rhodamine B by eutectic solvent extraction-liquid chromatography
  • Method for rapidly measuring rhodamine B by eutectic solvent extraction-liquid chromatography

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preparation example Construction

[0042] Preparation of deep eutectic solvent DES-2: Weigh 20g of choline chloride and 26.38g of glycerol into a 100mL reaction flask, raise the temperature to 90°C and stir until clear, then cool to room temperature for later use.

[0043] Preparation of the deep eutectic solvent DES-3: Weigh 20g of choline chloride and 39.57g of glycerol into a 100mL reaction flask, heat up to 90°C and stir until clear, then cool to room temperature for later use.

[0044] Step S3: Weigh the seasoning oil sample, add the deep eutectic solvent and alkane reagent described in step S2, perform extraction, remove the upper oil layer after centrifugation, wash the residue with alkane and use liquid chromatography to detect the chromatogram of the sample Figure; Wherein, the volume ratio of described deep eutectic solvent and alkane reagent is greater than 0.0025;

[0045] Step S4: Compare the chromatogram of the sample with the chromatogram of the standard working solution to determine whether Rhod...

Embodiment 1

[0047] Sample: Weigh 1g of chili oil into a 15mL centrifuge tube, add 1.0mL of deep eutectic solvent DES-1 and 5mL of n-hexane, extract by shaking for 10 minutes, centrifuge at 7500r / min for 2 minutes, absorb the oil layer with a plastic straw and discard Then add 5 mL of n-hexane, shake and wash for 1 minute, centrifuge at 7500r / min for 2 minutes, suck up the oil layer with a plastic straw and discard it. The remaining part of the deep eutectic solvent DES-1 was adjusted to 5.0 mL with methanol, vortexed and mixed, passed through a 0.22 μm organic filter membrane, and tested on the machine.

[0048]Spiked samples: Weigh 1 g of chili oil into a 15 mL centrifuge tube, add rhodamine B at a concentration level of 5.0 μg / kg, and prepare 6 spiked samples. Add 1.0mL of deep eutectic solvent DES-1 and 5mL of n-hexane to the spiked sample, shake the shaker for 10 minutes, extract at 10°C, centrifuge at 7500r / min for 2 minutes, absorb the upper oil layer with a plastic straw and discar...

Embodiment 2

[0054] Sample: Weigh 1g of pepper oil into a 15mL centrifuge tube, add 0.6mL of deep eutectic solvent DES-2 and 6mL of n-heptane, shake and extract for 15 minutes, centrifuge at 7500r / min for 3 minutes, absorb the above with a plastic straw Discard the oil layer, then add 5 mL of n-heptane, shake and wash for 1 minute, centrifuge at 7500 r / min for 2 minutes, absorb the upper oil layer with a plastic straw and discard. The remaining part of the deep eutectic solvent DES-2 was adjusted to 5.0 mL with methanol, vortexed and mixed, passed through a 0.22 μm organic filter membrane, and tested on the machine.

[0055] Spiked samples: Weigh 1 g of pepper oil into a 15 mL centrifuge tube, add rhodamine B at a concentration level of 5.0 μg / kg, and prepare 6 spiked samples. Add 0.6mL deep eutectic solvent DES-2 and 6mL n-heptane to the spiked sample respectively, shake the shaker for 15 minutes, extract at 30°C, centrifuge at 7500r / min for 3 minutes, use a plastic straw to absorb the oi...

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Abstract

The invention provides a method for rapidly measuring rhodamine B by a eutectic solvent extraction-liquid chromatography. The method includes the steps: preparing rhodamine B solution, diluting the solution into different concentrations of rhodamine B standard working solutions, detecting liquid chromatograms of the rhodamine B standard working solutions by the liquid chromatography, and making a calibration curve; preparing eutectic solvent; weighing flavoring oil samples, adding the eutectic solvent and alkane reagents to extract, removing an upper oil layer after centrifugation, and detecting by the liquid chromatography to obtain chromatograms of the samples after residue is washed by alkane; comparing the chromatograms of the samples and the chromatograms of the standard working solutions to determine the nature, and performing quantification according to the concentration of a peak area corresponding to a standard curve. The eutectic solvent comprises a hydrogen-bond acceptor compound and a hydrogen bond donor compound. The method is high in practicability, simple to operate and low in experimental cost, and complicated pretreatment processes are omitted.

Description

technical field [0001] The invention belongs to the technical field of detection of non-edible pigments in food, and in particular relates to a method for rapidly determining rhodamine B by deep eutectic solvent extraction liquid chromatography. Background technique [0002] Rhodamine B, also known as basic rose essence and flower pink, is a synthetic xanthene fluorescent dye, mainly used in the paper industry to dye waxy paper, typing paper, glossy paper, etc., in colored glass, special fireworks, etc. There are also applications in industries such as firecrackers. Because rhodamine B is easier to dye on hot pot bottoms, chili powder, seasoning oil, etc. than other edible water-soluble dyes, and it is not easy to fade and has low cost, so some unscrupulous traders dye these foods with rhodamine dyes. it is good. According to the International Agency for Research on Cancer (IARC) carcinogenic risk assessment of chemicals, ingestion, inhalation and skin contact with rhodami...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/74G01N30/86G01N30/06
CPCG01N30/06G01N30/74G01N30/8634
Inventor 李碧芳王韦达肖泽恩杜业刚李芸杨俊杨国武
Owner SHENZHEN ACAD OF METROLOGY & QUALITY INSPECTION
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