Method for detecting N-nitrosodimethylamine in meat products

A technology of dimethylnitrosamine and meat food, which is applied in the detection field of N-dimethylnitrosamine in meat food, can solve the problems of large NDMA loss, decreased accuracy, and lack of purification methods, and achieves Improved recovery rate, reduced loss, and ease of handling

Active Publication Date: 2019-06-07
广电计量检测(南宁)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the lack of sufficient purification means in the prior art, the concentration step is difficult to carry out when encountering high-

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  • Method for detecting N-nitrosodimethylamine in meat products
  • Method for detecting N-nitrosodimethylamine in meat products
  • Method for detecting N-nitrosodimethylamine in meat products

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Embodiment 1

[0031] Embodiment 1 A kind of detection method of N-dimethylnitrosamine in meat food

[0032] 1. Method

[0033] 1. Configuration of standard solution

[0034] Prepare a 10 μg / mL standard stock solution of NDMA in acetonitrile. Then use acetonitrile to prepare the standard working solution of response concentration and measure it on the machine. The concentration of the standard working solution is: 10, 20, 50, 100, 200, 500, 1000ng / mL.

[0035] 2. Sample pretreatment

[0036] Weigh 10g of bacon sample into a 50mL centrifuge tube, add 5mL of acetonitrile and 10mL of water, add 20mL of n-hexane, shake on a shaker at 300r / min for 20min, centrifuge at 4000r / min for 5min, and discard the n-hexane layer.

[0037] Add 15mL of dichloromethane and 10g of anhydrous sodium sulfate to the centrifuge tube, shake on a shaker at 300r / min for 20min, centrifuge at 4000r / min for 5min, take 10mL of the organic layer (containing about 2.5mL of acetonitrile, 7.5mL of dichloromethane ) in a c...

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Abstract

The invention discloses a method for detecting N-nitrosodimethylamine in meat products, which comprises the steps of S1, taking a sample to be detected, adding n-hexane, acetonitrile and water, oscillating, centrifuging and discarding the n-hexane layer; S2, adding dichloromethane and anhydrous sodium sulfate to the solution in the step S1, oscillating and centrifuging, taking an organic layer into a concentration bottle, adding ice water to a receiving bottle, carrying out rotary evaporation under the conditions of 350-360 mbar and 34-36 DEG C to remove dichloromethane, and if the remaining solution is greater than 1mL, adding dichloromethane for continuous rotary evaporation until the remaining solution is about 0.5-1mL; S3, removing the residue in the step S2, cleaning the concentrationbottle in the step S2 with a small amount of acetonitrile, n-hexane saturated with acetonitrile and n-hexane in sequence, mixing the washing liquid and the residue in the step S2, centrifuging, discarding the n-hexane layer, enabling the acetonitrile layer to be constant in volume to obtain the sample solution to be detected, and carrying out GC-MS determination. The pretreatment method applied by the invention is easy to operate, the high grease in the sample to be detected can be effectively removed, and the recovery rate of NDMA is significantly improved through improving the concentrationcondition at the same time.

Description

technical field [0001] The invention belongs to the technical field of food detection, and more specifically relates to a detection method for N-dimethylnitrosamine in meat food. Background technique [0002] Nitrosamines can cause tumors in almost all organs of the human body, among which digestive tract cancer is the most common. Mainly from the application of chemical fertilizers, nitrosamine compounds are commonly found in grains, milk, cheese, tobacco and alcohol, bacon, barbecue, sea fish, canned food and drinking water. There are many researches on the detection of nitrosamines at home and abroad. Nitrosamines in pickled aquatic products, children's latex mass spectrometry, drinking water, sausages, fruits, cigarettes, beer, cosmetics and other types of samples have been studied. Detectors for the determination of nitrosamines include mass spectrometry detectors, triple quadrupoles, thermal energy analyzers, nitrogen and phosphorus detectors, etc. Sample extraction...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 覃庆肖艳李硕牙东梅
Owner 广电计量检测(南宁)有限公司
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