Improved method for determination of sodium cyclamate in aquatic processed product
A processed product, cyclamate technology, applied in the field of aquatic product detection, can solve the problems of false positive test results, derivatization interference, low detection efficiency, etc.
Inactive Publication Date: 2017-01-18
MARINE FISHERIES RES INST OF ZHEJIANG
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Problems solved by technology
Among them, gas chromatography is a method widely used at present, GB / T 5009.97-2003 "Determination of sodium cyclamate in food", wherein the first method is gas chromatography, this method requires complex derivatization steps, the previous The processing steps are cumbersome, a large amount of n-hexane reagent is used, and the detection efficiency is low
At the same time, the derivatization in gas chromatography also has interference phenomenon. When analyzing the matrix rich in protein and alcohol, especially in the processing of aquatic products rich in protein and lipid, the derivatization interference is more serious, and the test results will appear false. positive
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[0021] An improved method for measuring cyclamate in processed aquatic products, comprising the steps of:
[0022] (1) Sample extraction: Weigh 2.00g of sample, place it in a 25mL centrifuge tube, add 10mL methanol aqueous solution (volume concentration 50%), mix well and vortex for 1min, place in a water bath at 60°C for 15min, then sonicate for 10min, centrifuge, Pour off the supernatant, use 10mL methanol aqueous solution to repeat the above operation to extract the residue, centrifuge once, combine the supernatant, and accurately dilute to 25mL to obtain the sample extract;
[0023] (2) Liquid chromatography-mass spectrometry detection: Take 1 mL of the sample extract, filter it into a sample bottle through a 0.22 μm organic filter membrane, perform liquid chromatography-mass spectrometry detection, then draw a standard working curve, and quantify it with the external standard method. The peak area was used to quantify cyclamate.
[0024] The liquid chromatography conditi...
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Abstract
The invention discloses an improved method for determination of sodium cyclamate in an aquatic processed product. An aquatic processed product sample is extracted by a methanol aqueous solution, is centrifuged, makes the volume constant, and is determined through an ultra-high performance liquid chromatography-mass spectrometry method. Through optimization of pretreatment and chromatographic conditions, sodium cyclamate has a good linear relationship in a range of 0.5-50 ng / mL, the correlation coefficient is 0.996 or more, the average recovery rate of the aquatic processed product sample is 81%-109%, the relative standard deviation is 2.2%-9.7%, and the quantitative detection limit is 0.01 mg / kg; the method is efficient, sensitive and accurate, and can be widely applied in determination of sodium cyclamate in the aquatic processed product.
Description
technical field [0001] The invention relates to the technical field of aquatic product detection, in particular to an improved method for determining cyclamate in processed aquatic products. Background technique [0002] Sodium cyclamate, also known as sodium cyclamate, is easily soluble in water. It is a low-calorie synthetic sweetener without any nutritional value, but its sweetness can reach 50-60 times that of white sugar. Flavor, with its low price and sweetness far exceeding white sugar, is widely used in pastries, condiments, beverages, preserves, etc. In recent years, the market circulation food monitoring of relevant departments has found that cyclamate in processed aquatic products is often detected. At the same time, research reports have found that excessive consumption of sweet vegetarian food may be carcinogenic, and it will be metabolized into cyclohexylamine in the body. These substances will have a toxic effect on the cardiovascular system and testicles, so...
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IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/88G01N30/06
Inventor 方益喻亮严忠雍祝银李子孟
Owner MARINE FISHERIES RES INST OF ZHEJIANG