Matrix dispersion solid phase extraction method for detection of plasticizer in animal and vegetable oil samples
A technology of animal and vegetable oils and dispersed solid phase, which is applied in the preparation of test samples, etc., can solve the problems of food contamination, cumbersome experimental process, time-consuming, etc., and achieve the effects of low cost, solvent saving, and simple experimental steps
Inactive Publication Date: 2012-08-01
TIANJIN CHUNFA BIO TECH GRP
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Problems solved by technology
[0002] In May 2011, according to media reports, some food additive manufacturers in Taiwan illegally added phthalate non-edible substances, and caused the food of downstream manufacturers using such food additives to be polluted
[0006] Although the relevant national departments have introduced plasticizer detection methods, among the existing detection methods, the pretreatment method for water phase samples is simple and easy, while for oily samples, gel filtration chromatography is usually used for sample processing. The method involves the use of a gel permeation chromatography separation system. The cost of this instrument is high, about RMB 300,000. Most enterprises and institutions do not have the conditions, and the experimental process of this method is cumbersome and time-consuming
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Embodiment 1
[0024] A kind of matrix dispersion solid phase extraction method that plasticizer detects in salad oil, comprises the steps:
[0025] Weigh 1g of solid phase extraction filler PSA (N-propylethylenediamine group bonded to silica gel) and place it in a stoppered glass centrifuge tube to obtain an extraction glass centrifuge tube. Weigh 0.5g of a salad oil sample and saturate it with 3ml of acetonitrile Dissolve in n-hexane, then extract twice with 5ml of acetonitrile saturated with n-hexane, centrifuge, combine the acetonitrile layer, transfer all the acetonitrile layers into the extraction glass centrifuge tube, shake fully, centrifuge at 6000r / min for 5min, take the supernatant and use GC / MS analysis. Select ion scanning, and conduct qualitative and quantitative analysis by establishing a standard curve. Parameter setting of GC / MS instrument: inlet temperature: 260°C splitless; column flow rate: 1.0mL / min; ionization voltage: 70eV; ion source temperature: 230°C; quadrupole t...
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The invention relates to a matrix dispersion solid phase extraction method for detection of plasticizer in animal and vegetable oil samples. The method comprises the following steps: (1) packing an extraction glass centrifuge tube: weighing 0.1-5g of solid phase extraction filler in a glass centrifuge tube with a stopper to obtain an extraction glass centrifuge tube; (2) weighing, dissolving and extracting: weighing 0.1-5g of an animal or vegetable oil sample, dissolving with 1-10ml acetonitrile saturated n-hexane, extracting with 1-10ml n-hexane saturated acetonitrile twice, centrifuging, combining acetonitrile layers as to-be-purified liquid; and (3) purifying: transferring the to-be-purified liquid into the extraction glass centrifuge tube, sufficiently shaking, centrifuging at a rotation speed of 1,000-10,000 r / min, collecting supernatant, analyzing with GC-MS (gas chromatography-mass spectrometry), establishing a standard curve with a standard sample, and carrying out quantitative and qualitative analysis. The method provided by the invention is especially suitable for rapid detection of phthalates in animal and vegetable oil samples.
Description
technical field [0001] The invention belongs to the field of analysis of trace organic matter in food matrices, in particular to a rapid extraction method for phthalates in animal and vegetable oil samples. Background technique [0002] In May 2011, according to media reports, some food additive manufacturers in Taiwan illegally added non-edible phthalates, which resulted in food contamination of downstream manufacturers using such food additives. According to the latest list released by the AQSIQ, as of June 6, the number of plasticizer-contaminated products in Taiwan has increased to 945, and the number of related companies involved has increased to 282. At the same time, this food safety incident is also spreading rapidly, and there are varying degrees of reactions in Hong Kong, the mainland and even overseas regions, which has aroused widespread concern from the government and society. The incident has now been notified to the World Health Organization and has become an...
Claims
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Inventor 邓莉戴东强
Owner TIANJIN CHUNFA BIO TECH GRP