A kind of detection method of unsaponifiable substance and grease ester type in fish oil

A detection method and saponification technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of requiring pretreatment steps and long detection time, and achieve the effect of shortening the detection time and simplifying the detection process

Active Publication Date: 2022-02-22
舟山新诺佳生物工程有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The main purpose of the present invention is to provide a kind of detection method of unsaponifiable matter and grease ester type in fish oil and grease, to solve the problem that the detection process of unsaponifiable matter in the prior art needs pretreatment step, detection time is long

Method used

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  • A kind of detection method of unsaponifiable substance and grease ester type in fish oil
  • A kind of detection method of unsaponifiable substance and grease ester type in fish oil
  • A kind of detection method of unsaponifiable substance and grease ester type in fish oil

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Preparation of sample solution: Take 0.15g of fish oil sample, accurately weigh it to 25mL, add mobile phase to dissolve and dilute to the mark, shake well; weigh 5 parts of 0.15g oil sample, accurately weigh to 25ml, add mobile phase to dissolve and Dilute to the mark, shake well, accurately measure 10 μL and inject it into the liquid chromatograph, and record the chromatogram.

[0041] Chromatographic conditions:

[0042] Chromatographic column: silica gel as filler (silica gel particle size 5μm, column length × inner diameter 250 × 4.6mm),

[0043] Detector: Differential Refractive Index Detector

[0044] Column temperature: 40°C

[0045] Mobile phase: n-hexane-isopropanol with a volume ratio of 90:10

[0046] Flow rate: 1.0ml / min,

[0047] Injection volume: 10μL

[0048] The resulting chromatograms are shown in figure 1 , where the chromatographic peak times are triglyceride type oil, ethyl ester type oil, 1.3-diester type oil, 1.2-diester type oil, unsaponifiab...

Embodiment 2

[0050] Preparation of sample solution: Take 0.15 g of the same fish oil sample as in Example 1, accurately weigh it to 25 mL, add n-hexane to dissolve and dilute to the mark, and shake well.

[0051] Chromatographic conditions:

[0052] Chromatographic column: silica gel as filler (silica gel particle size 5μm, column length × inner diameter 250 × 4.6mm),

[0053] Detector: Differential Refractive Index Detector

[0054] Column temperature: 25°C

[0055] Mobile phase: n-hexane-isopropanol with a volume ratio of 16:1

[0056] Flow rate: 1.0mLmin,

[0057] Injection volume: 10μL

[0058] The resulting chromatograms are shown in figure 2 .

[0059] After determination, all oil peaks and unsaponifiable matter have peaks, but compared with Example 1, the resolution is not good, and the peak type and analysis time are all poor.

Embodiment 3

[0061] The difference from Example 1 is that the column temperature is 25°C.

[0062] The detection spectrum of each peak is determined as image 3 , 1.3-diester type, 1.2-diester type grease peak shape is poor, not as good as embodiment 1.

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Abstract

The invention provides a method for detecting the types of unsaponifiable matter and grease esters in fish oil. The detection method includes: preparing fish oil oil solution; adopting high performance liquid chromatography to measure the oil solution, wherein the chromatographic conditions for determination include: the chromatographic column is selected from any one of silica gel column, amino column or cyano column; the mobile phase is A mixture of n-hexane and isopropanol. The present application utilizes the chromatographic column and mobile phase set for liquid chromatography detection, and the two match each other so that the unsaponifiable matter in fish oil and fat can be separated from other components, and some oils of different ester types in other components can also be separated, and then During detection, independent and complete characteristic peaks are obtained, and the detection of unsaponifiable matter and different types of fish oil lipid esters is completed. It can be seen that the present application does not require operations such as saponification and extraction of oils and fats, which simplifies the detection process and shortens the detection time, and there is no error caused by incomplete saponification.

Description

technical field [0001] The invention relates to the field of fish oil and fat quality evaluation, in particular to a method for detecting unsaponifiable matter and grease ester types in fish oil and fat. Background technique [0002] Unsaponifiable matter is the component in oils and fats that does not react with alkali except for fatty acids and glycerides, but is soluble in ether. Unsaponifiable matter includes sterols with high biological activity, high molecular weight fatty alcohols, hydrocarbons, pigments and fat-soluble vitamins, etc., which are insoluble in water but soluble in organic solvents such as ether. The method adopted in GB / T5535.2-2008 is to saponify the oil first, then extract the unsaponifiable matter with an organic solvent, and carry out Quantitative. The content of unsaponifiable matter in oil should be limited within a certain range. The higher the unsaponifiable content, the worse the oil quality. [0003] At present, the commonly used detection ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/32G01N30/36
CPCG01N30/02G01N30/36G01N30/06G01N30/32G01N2030/062G01N2030/027G01N2030/324
Inventor 劳敏军罗先庆宋江君董芮娟佘宽臣宋诗军
Owner 舟山新诺佳生物工程有限责任公司
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