Method for measuring phospholipid in lipid

A method of determination, oil technology, which is applied in the direction of material analysis by observing the influence of chemical indicators, and analysis by making materials undergo chemical reactions, which can solve problems such as cumbersome operation, long time-consuming carbonization, and difficult control of the carbonization process. Achieve the effect of simple and safe operation, shortening carbonization time and shortening ashing time

Inactive Publication Date: 2011-09-07
NORTHWEST UNIV(CN)
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

This method has the advantages of accuracy and high sensitivity, but has the following disadvantages: (1) It takes a long time to heat and carbonize in an electric furnace (refined oil takes 6-8 hours, and degummed oil takes 4-5 hours), and the carbonization process is not easy to control; (2) Add ZnO to convert into insoluble zinc phosphate, the follow-up operation is cumbersome, and the ashing temperature is limited
Chen Yong (China Oil, 2009,34(5):69-70) used a fan to prevent the sample from igniting when improving GB5537-2008, which can shorten the carbonization time by 2-3 hours, but this method is still time-consuming, and It does not solve the problem that the zinc phosphate produced by ashing is insoluble in water and needs to be boiled with acid to dissolve it

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  • Method for measuring phospholipid in lipid
  • Method for measuring phospholipid in lipid
  • Method for measuring phospholipid in lipid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1 precision test

[0034] Take 5 crucibles, add 3.0g of Zanthoxylum bungeanum seed oil to each, then add 1.0mL of concentrated sulfuric acid and 3.0g of solid potassium hydroxide, place on a 600W electric furnace and heat for 15min to carbonize until the oil sample is solid, and then put it into a programmed heating Ashing in a furnace at 700°C for 1.5h, cooling to room temperature, dissolving and filtering with 50mL hot water, after cooling, adjust the pH value to about 3 with 1:1 hydrochloric acid, and set the volume to 100mL;

[0035] Pipette 10 mL of the above test solution into a 50 mL colorimetric tube, add 8 mL of hydrazine sulfate solution and 2 mL of sodium molybdate solution, stopper, shake well, remove the plug, place the colorimetric tube in a boiling water bath for 10 min, take it out, Cool to room temperature, dilute to the mark with water, shake well, let it stand for 10 min, and measure its absorbance with a spectrophotometer at 650 nm. Subst...

Embodiment 2

[0038] Embodiment 2 Recovery test

[0039] Prepare phosphorus standard solutions of low, medium and high concentrations respectively, add them to Fulinmen first-grade refined soybean oil, and measure the phosphorus content therein after mixing. The operating conditions are the same as those in Example 1. See Tables 2, 3, and 4 for specific experimental data;

[0040] Table 2 Experimental results of recovery at high concentration (with P content about 0.8 mg)

[0041]

[0042] Table 3 Experimental results of recovery at medium concentration (containing about 0.4 mg of P)

[0043]

[0044] Table 4 Experimental results of recovery at low concentration (with P content about 0.1 mg)

[0045]

[0046] As can be seen from Tables 2, 3, and 4, the recovery rate is between 97.57% and 101.88%, and the accuracy of the present invention meets the detection requirements.

[0047] Comparative experiment Comparative experiment with GB5537-2008

[0048] Repeat the above measuremen...

Embodiment 3

[0058] Example 3 Detection of Phospholipid Content in Tung Oil Crude Oil

[0059] ( ) Preparation of phosphate standard stock solution: Weigh 0.4387 g of potassium dihydrogen phosphate dried for 24 hours, dissolve with water and dilute to 1000mL;

[0060] ( ) Preparation of hydrazine sulfate solution: dissolve 0.15 g hydrazine sulfate in 1L water to obtain 0.015% hydrazine sulfate solution;

[0061] ( ) Preparation of sodium molybdate dilute sulfuric acid solution: Measure 140mL of concentrated sulfuric acid and pour it into 300mL of water, cool to room temperature, add 12.5 g of sodium molybdate, dissolve and dilute to 500mL with water, shake well, and let it stand for 24 hours for later use;

[0062] (4) Preparation of hydrochloric acid solution: dissolve 37% concentrated hydrochloric acid in equal volume of water;

[0063] (5) Draw the standard curve: Add 0, 1, 2, 4, 6, 8 mL of phosphate standard solution to 6 colorimetric tubes, add water to make up to 10 mL; then a...

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Abstract

The invention discloses a method for measuring phospholipid in lipid, and the method comprises the following steps: carbonizing, ashing and dissolving of lipid; and molybdenum blue colorimetry measurement of phosphorus, wherein the lipid is carbonized by adding concentrated sulphuric acid, and a hydroxide, a carbonate or a bicarbonate of an alkali metal. In the invention, the concentrated sulphuric acid is used for pre-carbonizing, and alkali is added for reacting, so that the carbonization of different amounts of various lipids can be completed within 15 minutes, splashing and combustion generated in a direct electric furnace heating carbonization procedure are prevented, and the carbonization time is shortened; the hydroxide, carbonate or bicarbonate of the alkali metal is used for displacing ZnO, so that the soluble phosphate with higher thermal decomposition temperature is generated, and the ashing time is shortened; and the ashed product can be dissolved and filtered directly, sothat the following operations are simpler and safer.

Description

technical field [0001] The invention relates to a method for determining phospholipids in oil. Background technique [0002] During the oil refining process, the phospholipids in the crude oil will cause foaming, color reversion and oxidation stability of the oil, affecting the flavor of the oil, and the phospholipid-rich crude oil foot is the main raw material for the production of phospholipid health products. The high phospholipid feedstock oil in the biodiesel production process will lead to severe inactivation of lipase. The phospholipid content in liposome is an important index to measure its stability. Therefore, in the production of oil products, phosphorus content is a very important detection index. [0003] At present, the detection methods of phospholipids include colorimetric method, turbidimetric method, gravimetric method, TLC, HPLC, IR, NMR and so on. Nephelometric and gravimetric methods have limited application due to low detection accuracy; TLC method i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/78
Inventor 陈斌赵万里马晓迅李蓉
Owner NORTHWEST UNIV(CN)
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