Detection method for liquid chromatography tandem mass spectrometry of semi carbazide

A detection method, liquid chromatography technology, which is applied in the detection field of food pollutants, can solve the problems such as the lack of SEM detection method standards, and achieve the effects of rapid detection, high sensitivity and low detection limit

Inactive Publication Date: 2015-04-29
苏州市产品质量监督检验所 +2
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no standard for the detection method

Method used

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  • Detection method for liquid chromatography tandem mass spectrometry of semi carbazide
  • Detection method for liquid chromatography tandem mass spectrometry of semi carbazide
  • Detection method for liquid chromatography tandem mass spectrometry of semi carbazide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Accurately weigh 0.01g (accurate to 0.0001g) of the SEM standard substance, place it in a 10mL brown volumetric flask, dissolve it with a small amount of methanol, and then dilute to 10mL with methanol to prepare a 1000mg / L SEM stock solution. Weigh 1.0g (accurate to 0.0001g) of 6 negative blank flours into a 50mL centrifuge tube, add SEM standard solution respectively, so that the final concentrations are 1.0, 2.5, 5.0, 10.0, 30.0, 50.0 μg / kg respectively, according to the protocol ( 1) after sample pretreatment, measure by the detection condition of scheme (2), carry out linear regression to concentration X (mg / L) with peak area (Y), draw standard curve ( figure 1 ), by continuously reducing the concentration of the standard solution, the concentration at which the signal-to-noise ratio is 3 is taken as the lowest detection limit. The function relationship of the standard curve is: Y=0.5885+0.1871X, and the correlation coefficient is R 2 =0.9995, the lowest detection...

Embodiment 2

[0020] Accurately weigh 1.0g (accurate to 0.0001g) of 3 parts of blank flour as the matrix, add SEM standard solution respectively, so that the SEM content in the flour is 10.0, 20.0, 40.0μg / kg respectively, follow the sample pretreatment steps in the scheme (1) For processing, do 3 parallel tests at each concentration level, detect according to the detection conditions of the scheme (2), and measure the recovery rate and precision of the method. The analysis results are shown in Table 1. The recovery rate was 89.46%-101.20%, and the relative standard deviation was 2.48%-4.71%, which indicated that the method established in this study was reliable.

[0021] Table 1 SEM recovery and precision determination results of spiked flour

[0022]

Embodiment 3

[0024] Through the SEM content detection of 9 different types of noodle products, the samples were processed according to the sample pretreatment steps in the scheme (1), and the detection was carried out according to the detection conditions of the scheme (2). The measurement results are shown in Table 2.

[0025] Table 2 Content of SEM in commercially available flour products

[0026]

[0027]

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Abstract

The invention belongs to the field of detection of food contaminant semi carbazide (SEM). The method comprises the following steps: adding 0.2 mol/L hydrochloric acid hydrolysis solution, a 2-nitrobenzaldehyde derivating agent and an internal standard substance into a sample to perform SEM hydrolysis and derivatization, centrifuging, taking supernate, adjusting the pH value of the supernate to be neutral, allowing the supernate to pass a Poly-Sery HLB solid-phase extraction small column, performing eluting through methyl alcohol, gathering eluted liquid nitrogen, blowing the eluted liquid nitrogen to be dry, fixing the volume through 10 percent of an acetonitrile solution, filtering the eluted liquid nitrogen through a 0.22-micron film, and allowing the eluted liquid nitrogen to enter a liquid chromatography tandem mass spectrometer to be detected. Liquid chromatography adopts an XBirdge BEH Amide normal-phase chromatographic column, and acetonitrile and pure water of which volume ratio is 80 to 20 serve as mobile phases; mass spectrometry adopts an electrospray positive ion mode and a multi-reaction monitoring scanning way. The lowest detection limit is 0.01 microgram/kg. The invention discloses an SEM detection method with high detection speed, high sensitivity and low detection cost.

Description

technical field [0001] The invention belongs to the detection field of food pollutants, and is a method for rapidly and accurately detecting semicarbazide by using liquid chromatography tandem mass spectrometry. Background technique [0002] As a raw material for organic synthesis, semicarbazide (SEM) is well known because it is a characteristic metabolite of the veterinary drug nitrofurazone. It was subsequently found that the flour improver azodicarbonamide (ADA) could be transformed into SEM during flour processing. In addition, foaming agent ADA is added to the plastic gasket with polyvinyl chloride (PVC) as the main raw material. In the process of sealing glass bottles and disinfection treatment, after high-temperature heating conditions, the foaming agent thermally decomposes to generate SEM. [0003] A series of studies on the toxicity of SEM have been carried out at home and abroad. The toxicology experiments show that SEM is carcinogenic and mutagenic, and can caus...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 李培卫荣陈英丁洪流许亮袁丽红姚卫蓉
Owner 苏州市产品质量监督检验所
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