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Method for rapid analysis of phospholipid based on solvent extraction coupled FTIR (Fourier transform infrared spectroscopy)

A rapid analysis, phospholipid technology, applied in the analysis of materials, material analysis by optical means, preparation of test samples, etc., can solve the problems of large sample capacity, high cost, not suitable for samples with low phospholipid content, etc. The effect of good accuracy, high precision and simple operation

Active Publication Date: 2012-07-04
浙江吉美食品科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, to establish an accurate quantitative model, a large sample volume is often required, the cost is high, and it is not suitable for samples with low phospholipid content (<1000ppm)

Method used

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  • Method for rapid analysis of phospholipid based on solvent extraction coupled FTIR (Fourier transform infrared spectroscopy)
  • Method for rapid analysis of phospholipid based on solvent extraction coupled FTIR (Fourier transform infrared spectroscopy)
  • Method for rapid analysis of phospholipid based on solvent extraction coupled FTIR (Fourier transform infrared spectroscopy)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. Preparation of Standard Curve

[0026] (1) Take Sigma spectroscopic grade acetonitrile and methanol respectively, prepare acetonitrile methanol mixture with a volume ratio of 1:1 as a solvent, and use 25 μm CaF2 Sample cell, scan times 32, resolution 0.5cm -1 , spectral range 4000 ~ 400cm -1 Record the original spectrum S_0; (2) take an appropriate amount of the solvent described in step (1) respectively, add phosphatidylcholine (PC) standard substance (Sigma company, the United States) to prepare 20, 50, 100, 200, 500, 1000, 1500 , 2000, the phospholipid standard solution of 5000ppm, utilize infrared spectrometer analyzer (Tensor27, U.S. Bruker spectral instrument company), adopt 25 μ m CaF 2 Sample cell, scan times 32, resolution 0.5cm -1 , spectral range 4000 ~ 400cm -1 Record the spectra of the series of standard sample solutions, which are respectively recorded as S_std_1, S_std_2, S_std_3, S_std_4, S_std_5, S_std_6, S_std_7, S_std_8, S_std_9, and then do the...

Embodiment 2

[0030] Embodiment 2 Solvent extraction coupling FTIR analysis method for phospholipid content in edible oil samples

[0031] (1) Dephospholipid treatment of oil

[0032] Take 200g of silica gel G (200-300 mesh, Qingdao Ocean Chemical Co., Ltd.) activated at 105°C for 2h and fill it in a 3mm×400mm glass chromatography column to prepare a silica gel chromatography column; respectively take 50-100g of refined soybean oil (Arowana ) and canola oil (Arowana), respectively added to the above-mentioned silica gel chromatography column, vacuum adsorption, and the effluent was collected to obtain refined soybean oil degummed oil and canola oil degummed oil respectively.

[0033] (2) Solvent extraction coupling FTIR analysis method for phospholipid content in edible oil samples

[0034] (a) Accurately pipette 10mL (9.20g) of refined soybean oil sample, put it into a 30mL stoppered glass tube, add 20mL of acetonitrile / methanol 1:1 (volume ratio) mixture (15.80g), seal, vigorously mix an...

Embodiment 3

[0035] Embodiment 3 Different organic solvent extraction analyzes the comparison of soybean oil phospholipid content

[0036] A suitable organic solvent should firstly have sufficient dissolving power for phospholipids to ensure the complete extraction of phospholipids, and at the same time have as low a solubility as possible for interfering substances such as triglycerides to reduce spectral interference. Accordingly, under the condition that the organic solvent / grease volume ratio is 3: 1, the extraction effects of spectrally pure polar solvents DMSO, methanol, ethanol, and acetonitrile were compared respectively. Other operations were the same as in Example 1, and the results are shown in Table 2.

[0037] Accurately pipette 10 mL of refined soybean oil degummed oil described in Example 2 as a sample, place it in a 30 mL stoppered glass tube, add 20 mL of different organic solvents (see Table 2), seal, vigorously mix and extract for 1 min, centrifuge at 4000 rpm for 10 min,...

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Abstract

The invention discloses a method for rapid analysis of phospholipid based on solvent extraction coupled FTIR (Fourier transform infrared spectroscopy), which comprises the following steps: (1) extracting grease A containing 200-5000 ppm of phospholipid with an organic solvent A, collecting upper layer extractive solution A, and detecting infrared spectrum in a spectrum range of 4,000-400cm<-1>, marked as S_5; (2) treating grease B same as the grease A with a silica gel column to obtain degummed oil B, extracting the degummed oil B with an organic solvent B, collecting upper layer extractive solution B, and detecting infrared spectrum in a spectrum range of 4,000-400cm<-1>, marked as S_4; and (3) carrying out difference spectrometry analysis of S_4 and S_5, and obtaining the concentration of phospholipid in the grease A according to a phospholipid standard curve. The method of the invention is simple and safe to operation, environment-friendly, can continuously operate, has high precision and sensitivity, and is suitable for analysis of trace phospholipid in edible oil.

Description

(1) Technical field [0001] The invention relates to a method for measuring phospholipids, in particular to a method for rapidly analyzing phospholipids based on solvent extraction coupled with FTIR. (2) Background technology [0002] Phospholipids, as one of the dietary components, have many physiological functions for the human body, such as regulating fat metabolism, transporting essential fatty acids, and preventing diseases such as arteriosclerosis, hypertension, thrombosis, and ulcers. Phospholipids are mainly derived from vegetable oils, for example, the content of phospholipids in soybean crude oil is about 0.5-2%. But in terms of processing technology, the existence of phospholipids in vegetable oil is unfavorable, it will increase the loss of neutral oil in the deacidification process and the amount of bleaching clay, and it is easy to cause poisoning of the hydrogenation catalyst. If the phospholipids in refined oil are too high, it is easy to oxidize and affect t...

Claims

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Application Information

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IPC IPC(8): G01N21/35G01N1/28G01N21/3563G01N21/3577
Inventor 孟祥河潘秋月
Owner 浙江吉美食品科技有限公司
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