Liquid chromatographic analysis method for detecting acrylamide in fried food
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A liquid chromatographic analysis and fried food technology, which is applied in the field of liquid chromatographic analysis for detecting acrylamide in fried food, can solve the problems of low detection limit, long operation period, high price, etc., and achieves stable peak shape and baseline , The effect of fast detection and low limit of quantification
Inactive Publication Date: 2017-03-29
HUBEI UNIV OF TECH
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These two methods are detected by mass spectrometry, with accurate quantification and low detection limit, but the price is too expensive, which is not suitable for popularization and use in ordinary laboratories, and bromination derivatization is required in the early stage of GC-MS, and the sample processing operation cycle is long, and derivatization Chemical reagents are highly toxic, and at the same time, due to the weak retention of acrylamide during LC-MS / MS detection, the peaks of impurities coexisting in food will cover it, and in mass spectrometry detection, acrylamide has the same mass-to-charge ratio. ions, thus affecting the detection accuracy
In the prior art, the content of acrylamide in food was determined by reversed-phase high-performance liquid chromatography and normal-phase high-performance liquid chromatography, and the detection limits reached 4.0 μg·kg-1 and 10.0 μg·L-1 respectively, but It is more complicated, and the promotion of normal phase chromatography in the laboratory is relatively small
[0004] The existing national standard analysis and detection method (GB5009.204-2014) has complex steps, takes more than 10 minutes, takes a long time, and requires derivation; using the standard addition method, only one sample can be processed at a time; the limit of quantification is 10 μg / kg
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Embodiment 1
[0032] 1) Weigh 2.0 g of ground and crushed commercially available French fries, place them in a 20 mL polytetrafluoroethylene centrifuge tube, add 3 levels of acrylamide standard solution, and let stand for 10 min;
[0033] 2) Add 10 mL of n-hexane to the resting liquid obtained in step 1), vortex and shake for 1 min and let stand for 10 min, discard the petroleum ether layer, blow dry with nitrogen at 40±1°C, and repeat the above-mentioned n-hexane degreasing process once;
[0034] 3) Add 14 mL of deionized water to the degreased sample in step 2), vortex and shake for half a minute, then put it into a constant temperature oscillator and shake at 60°C for 30 minutes, then take it out, and then ultrasonically shake the obtained solution for 20 minutes;
[0035] 4) Add 0.5 mL each of Carrez I and Carrez II reagents to the shaking solution obtained in step 3), let stand for 10 minutes to remove protein, centrifuge at 4°C and 11,000 rpm for 20 minutes at high speed, take 2 mL of ...
Embodiment 2
[0039] Embodiment 2, with embodiment 1, the difference is,
[0040] 1) Weigh 2.0 g of ground and pulverized commercially available fried chicken legs, place them in a 20 mL polytetrafluoroethylene centrifuge tube, add 3 levels of acrylamide standard solution, and let stand for 10 min.
Embodiment 3
[0041] Embodiment 3, with embodiment 1, the difference is,
[0042] 1) Weigh 2.0 g of ground and pulverized commercially available sweet potato cakes, place them in a 20 mL polytetrafluoroethylene centrifuge tube, add 3 levels of acrylamide standard solution, and let stand for 10 min.
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Abstract
The invention relates to a liquid chromatographic analysis method for detecting acrylamide in fried food. The liquid chromatographic analysis method for detecting acrylamide in fried food comprises the following steps: taking ground and pulverized fried food, adding an acrylamide standard substance solution, adding n-hexane, carrying out eddy vibration, removing a petroleum ether layer, adding deionized water, carrying out eddy vibration and constant-temperature oscillation, carrying out ultrasonic oscillation, adding Carrez reagents Carrez I and Carrez II to remove protein, centrifuging at high speed, enabling supernate to pass through activated SPE small columns, and filtering to obtain a test article solution; and analyzing the test article solution by using a liquid chromatography. The acrylamide is heated and extracted with deionized water and is ultrasonically extracted, the extracting rate is 98.2%, and RSD is equal to 2.83%; the deionized water is safe and non-toxic, and is low in price; and the detection limit and the limit of quantitation are low, the detection limit is 0.002 mu g.mL-1, and the limit of quantitation is 0.005 mu g.mL-1. The liquid chromatographic analysis method is rapid, accurate, efficient and safe, and can accurately detect the content of the acrylamide in the fried food.
Description
technical field [0001] The invention relates to an analysis technology for acrylamide in fried food, in particular to a liquid chromatography analysis method for detecting acrylamide in fried food. Background technique [0002] Acrylamide has strong permeability and can quickly enter the human body through the respiratory tract, digestive tract, skin and mucous membranes to cause poisoning. Animal experiments and long-term exposure experiments show that it mainly has neurotoxicity, reproductive toxicity, genotoxicity and teratogenicity. As early as 1994, the International Agency for Research on Cancer listed acrylamide as a Group 2A "probable human carcinogen". [0003] At present, the methods for detecting acrylamide in the world are mainly through solid phase extraction column purification and 13 C or 2 H-labeled acrylamide was determined by isotope dilution gas chromatography-mass spectrometry (GC-MS) and high-performance liquid chromatography-mass spectrometry (HPLC-M...
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