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Method for detecting mineral oil in edible oil and fat by virtue of gas chromatograph-mass spectrometer

A gas chromatography and edible oil technology, applied in the field of edible oil detection, can solve the problems of false positives, inability to quantitatively detect, and high detection limit of the detection method, and achieve the effect of low detection limit and high sensitivity

Active Publication Date: 2015-08-12
中粮工科(西安)国际工程有限公司
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Problems solved by technology

[0005] The purpose of the present invention is to provide a method for detecting mineral oil in edible oils and fats by gas chromatography-mass spectrometry, which can effectively solve the problems of high detection limit, serious false positives, and inability to quantitatively detect the present detection method.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Accurately weigh 0.5g oil sample, the weighing should be accurate to 0.001g;

[0027] (2) Add 5mL n-hexane to the sample to dilute, use a screw shaker to oscillate for 2 minutes; centrifuge for 3 minutes at a speed of 4000r / min;

[0028] (3) Filter the sample through an organic filter membrane with 0.22μm pore size or filter the sample through an SPE cartridge with Pas powder as the filler;

[0029] (4) The oil sample pretreated by steps 1 to 3 is injected through the sampler and detected by GC-MS;

[0030] (5) Calculate the total area of ​​the mineral oil peaks in the GC-MS spectrum according to the area addition method, and then compare the mineral oil standard curve to calculate the mineral oil content in the oil sample as A 1 ;

[0031] (6) Blank test: Except that the oil sample is not weighed, it is carried out in steps 2 to 5, and the mineral oil content in the blank sample is calculated as A 0 ;

[0032] (7) Parallel test: According to steps 1 to 5, perform parallel tes...

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Abstract

The invention discloses a method for detecting mineral oil in edible oil and fat by virtue of gas chromatograph-mass spectrometer. The method comprises the following steps: firstly, accurately weighing 0.5g of a sample (the weighing is precise to be 0.001g), and preparing a blank sample; secondly, diluting the sample with 5mL of n-hexane and oscillating by virtue of a spiral oscillator for 2min, and processing with a centrifuge for 3min at the rotating speed of 4000r / min; then, filtering the sample by virtue of an organic filter membrane which is 0.22 microns in aperture or filtering and purifying the sample by virtue of a solid phase extraction (SPE) small column; and finally, injecting the preprocessed sample through a sample injector, calculating total peak area of mineral oil in a gas chromatograph-mass spectrometer (GC-MS) map according to an area addition method, and calculating the content of the mineral oil in an oil discharging sample in accordance with a mineral oil standard curve. The method disclosed by the invention can be used for effectively solving the problems of a current detection method that detection limit is high, false positive status is severe, and quantitative detection fails and the like.

Description

Technical field [0001] The invention belongs to the field of edible oil detection, and specifically relates to a method for detecting mineral oil in edible oil by using a gas chromatography-mass spectrometer. Background technique [0002] In recent years, incidents of edible fats being contaminated with mineral oil have occurred from time to time. Mineral oil contains many toxic substances, most of which cause harm to living organisms. And these toxic components can reach the human body through the enrichment of the food chain, affecting health and safety. Mineral oil has an impact on the digestive system, nervous system, and respiratory system in the human body, and can cause skin allergies, cancer, deformities and other diseases. Therefore, mineral oil pollution has attracted great attention in China and the world. [0003] However, the detection limit of the method specified in my country's national standard GB / T 5009.37-2003 "Methods for the analysis of hygienic standards for...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 曹万新张闽王月华范明亮王萍李文娟张骊史宣明陈燕
Owner 中粮工科(西安)国际工程有限公司