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Analysis method of free sterol components in edible oil sample and swill-cooked dirty oil identification method

An analysis method and edible oil technology, applied in the direction of analysis materials, material separation, measuring devices, etc., can solve the problems of insufficient chromatographic separation ability, excessive organic solvent, consumption, etc., achieve strong chromatographic separation ability, less organic solvent consumption, The effect of high data collection frequency

Inactive Publication Date: 2015-01-07
INST OF OIL CROPS RES CHINESE ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this type of method, the samples need to undergo complex pretreatment before sample injection, such as saponification of oil, extraction of unsaponifiable matter, alumina column chromatography, thin layer chromatography, etc. The process is time-consuming and laborious, and requires a lot of consumption organic solvents, which cannot meet the daily environmental protection and fast requirements (ISO 12228:1999, Food Chemistry 2013, 136, 251-258, Food Research International, 2011, 44, 103-108)
In addition, GC-FID is often insufficient in the analysis of sterols with low content in edible oil samples, and is particularly susceptible to the interference of the matrix in the sample, and the quantitative error of trace sterols is relatively large; at the same time, one-dimensional gas chromatography and comprehensive two-dimensional gas chromatography Compared with chromatography, its chromatographic separation ability is insufficient, and it often cannot achieve satisfactory separation effect for some isomers of sterols, which brings interference to the precise quantification of individual sterols

Method used

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  • Analysis method of free sterol components in edible oil sample and swill-cooked dirty oil identification method
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  • Analysis method of free sterol components in edible oil sample and swill-cooked dirty oil identification method

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Example 1: Qualitative and quantitative analysis of free sterols in edible oil samples

[0045] (1) Preparation of sample solution: Accurately weigh 0.05 g (accurate to 4 decimal places) of edible oil samples (soybean oil, rapeseed oil, peanut oil, sunflower oil, corn oil and gutter oil), and add 20 μg gallbladder The stanol internal standard was then dissolved in 5mL of n-hexane, vortexed evenly, and set aside.

[0046] (2) Sample loading: Inject the uniformly oscillating sample solution in (1) into the activated SPE column, control the flow rate to 1.2-1.6mL / min, and discard the effluent; the SPE column is 0.5mg / 6mL Silica gel column, the activation is to weigh 1.0g of anhydrous sodium sulfate and add it to the top of the SPE column, then activate it with 10-15mL n-hexane solution, the flow rate is 1.0-2.0mL / min, and discard the effluent;

[0047] (3) Rinse: use 10 mL of diethyl ether n-hexane solution (v / v) with a volume percentage concentration of 5-6% for rinsing,...

Embodiment 2

[0067] Example 2: Analysis of free sterol components in waste oil samples and identification of waste oil

[0068] Accurately weigh 0.06g (accurate to 4 decimal places) waste oil and 2 rapeseed oil samples each, add 20μg cholestanol internal standard, then dissolve with 6mL n-hexane, vortex and oscillate evenly to obtain the sample solution , followed by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry analysis. Obtain qualitative and quantitative results. The analysis steps are basically the same as in Example 1, except that the selected comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry analysis conditions are slightly different, specifically: the inlet temperature is set at 310 ° C, with helium as the carrier gas, and the flow rate is 0.9mL / min. The injection volume was 2 μL, and the split ratio was 15:1. The heating program of the one-dimensional furnace oven is as follows: the initial temperature is 190°C,...

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Abstract

The invention relates to an analysis method of free sterol components in an edible oil sample and a swill-cooked dirty oil identification method. The analysis method comprises the following steps: carrying out solid phase extraction on the edible oil sample to be tested to separate out the free sterol in the sample, carrying out silylation derivatization on the free sterol, injecting a comprehensive two-dimensional gas chromatography-time-of-flight mass spectrum into the free sterol for detection, and realizing qualitative and quantitative analysis on the free sterol components in the edible oil sample. Compared with a traditional sterol compound analysis method, the analysis method has the characteristics of high sensitiveness, rapidness and high efficiency, an adulterated edible oil identification and swill-cooked dirty oil identification method is established through analyzing a proportional relation between phytosterol in cholesterol in different edible oil as well as a proportional relation between the cholesterol and other specific phytosterol, and the authenticity identification of the edible oil and the identification of the swill-cooked dirty oil can be realized.

Description

technical field [0001] The invention relates to a method for analyzing free sterol components in edible oil samples and a method for identifying waste oil, which can be used for qualitative and quantitative analysis of free phytosterols and cholesterol in edible oil, and can identify waste oil based on discriminant factors. Background technique [0002] The quality and safety of edible oil has become a hot issue of public concern. "Gutter oil" in a broad sense includes waste oil, swill oil (swill oil), old frying oil, and fats and oils refined from animal waste. Some refined "gutter oils" are not significantly different from normal edible oils in terms of physical and chemical indicators such as color, smell, peroxide value, acid value, and iodine value, which has brought great challenges to the quality supervision and safety management of edible oils. Difficulties. Due to the temptation of profits, some unscrupulous traders sell refined "waste oil" as edible oil or add it...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/08
Inventor 李培武徐宝成张良晓马飞张奇王秀嫔张文
Owner INST OF OIL CROPS RES CHINESE ACAD OF AGRI SCI
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