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Analysis and detection method for effectively screening phospholipid in krill oil

A detection method and technology for krill oil, applied in analytical materials, measurement devices, material separation, etc., can solve problems such as interference, difficulty in non-targeted screening, complex big data, etc.

Pending Publication Date: 2020-10-23
ZHEJIANG GONGSHANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the complexity of "omics" big data, this method is easily interfered by saturated or short-chain phospholipids during the detection process, making it non-target for variable molecular weight EPA-type structural phospholipids and DHA-type structural phospholipids. It is difficult to filter

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  • Analysis and detection method for effectively screening phospholipid in krill oil
  • Analysis and detection method for effectively screening phospholipid in krill oil
  • Analysis and detection method for effectively screening phospholipid in krill oil

Examples

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experiment example 1

[0057] Experimental example 1: configure phospholipid standard solution according to the method described in the present invention and detect, utilize the induced collision dissociation (CID) method in liquid chromatography mass spectrometry during detection to detect after phospholipid standard solution is crushed. Test results such as Figure 1-3 As shown, when the product ionic strengths of EPA-type structural phospholipids and DHA-type structural phospholipids are at m / z301.2 and m / z327.2, the EPA-type structure can be stably detected by precursor ion scanning-liquid chromatography-mass spectrometry Non-targeted screening of phospholipids and DHA-type structural phospholipids.

[0058] During the detection, the collision voltage and the declustering voltage in the mass spectrometry conditions are respectively subjected to an orthogonal test, and then the dissociation efficiency of the EPA chain and the DHA chain in each phospholipid is detected. Test results such as Fig...

experiment example 2

[0069] Experimental example 2: In this experimental example, the chromatogram and retention time of the blank sample and the chemical standard solution are compared, and the calibration curve of each phospholipid under a series of concentration gradients is established at the same time, and the peak area and the analyte are plotted with a weighting factor of 1 / x Concentration graph. The results are shown in Table 2. For each phospholipid standard, the calibration curve is linear from the LOQ to the concentration range of 1000 μg / mL, and the average correlation coefficient is 0.9978-0.9993, which indicates that the peak area (y) and the phospholipid concentration (x , μg / mL) showed a good linear relationship. Using the standard addition method, the method detection limit (LOD) and quantification limit (LOQ) of the analyte were determined according to 3 and 10 times the signal-to-noise ratio (S / N), respectively, PL EPA / DHA The LOD≤4.02μg / mL, LOQ≤13.4μg / mL, the results show that...

experiment example 3

[0073] Experimental example 3: In this experimental example, the precursor ion scanning-liquid chromatography-mass spectrometry method of the present invention is compared with conventional liquid chromatography-mass spectrometry, shotgun method and rapid evaporation ionization mass spectrometry. Test result is as shown in table 3, precursor ion scanning-liquid chromatography mass spectrometry of the present invention can detect 33 kinds of PL EPA / DHA Molecular species, including 16 PCs E / D , 11 types of PE E / D and 6 kinds of PI E / D . A total of 11 PCs were detected by normal phase liquid chromatography-mass spectrometry E / D , but because the system is in positive ion mode, no phospholipid species of PE and PI were found. A total of 13 PL species were detected by fast evaporation ionization mass spectrometry EPA / DHA numerator, where PC E / D or PE E / D 6 types each, PI E / D 6 species, PA E / D 1 species. The shotgun method detected a total of 15 PCs E / D molecular. By the...

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Abstract

The invention discloses an analysis and detection method for effectively screening phospholipid in krill oil. The method comprises the following steps: taking krill powder, uniformly grinding, addinginto a trichloromethane-methanol mixed solution, and uniformly oscillating at room temperature to obtain an extracting solution A; performing ultrasonic treatment on the extracting solution A, centrifuging the mixture, and collecting a lower-layer organic phase and centrifuged residues to obtain an organic phase B and residues C; re-extracting the residue C with trichloromethane for multiple times, and collecting a lower-layer organic phase to obtain an organic phase D; mixing the organic phase B with the organic phase D to obtain an e1 extracting solution, blow-drying the e1 extracting solution, fixing the volume with acetonitrile, and filtering with an organic filter membrane to obtain a to-be-detected solution E; and finally, detecting the to-be-detected solution E through a hydrophilicinteraction liquid chromatography-mass spectrometry method in a precursor ion scanning mode. The method can realize non-targeted screening of phospholipid in krill oil, and has the characteristics ofhigh detection efficiency, high detection accuracy and high resolution.

Description

technical field [0001] The invention relates to a detection method for krill oil, in particular to an analysis and detection method for effectively screening phospholipids in krill oil. Background technique [0002] Antarctic krill is one of the most abundant organisms found in the waters of Antarctica in the Antarctic Ocean. It has great potential and application prospects, and its krill oil is often used as a substitute for fish oil in the market. Krill oil, which is rich in eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA), differs from other biological sources of omega-3 fatty acids in that krill oil is found in the sn- Position 2 contains high levels of omega-3 fatty acid acyl chains, and omega-3 fatty acids in fish oil are usually in triglyceride or ethyl ester form. Because EPA-type structural phospholipids and DHA-type structural phospholipids can easily bind to cell membranes and be absorbed by the intestines, thereby reducing cardiovascular risk, improvin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N30/7266G01N2030/062
Inventor 沈清俞喜娜朱小芳
Owner ZHEJIANG GONGSHANG UNIVERSITY
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