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High performance liquid chromatography-tandem mass spectrometry detection method of plasticizer in sugar

A technology of high performance liquid chromatography and tandem mass spectrometry, which is applied in the field of detecting plasticizers and achieves the effects of fast detection time and simple detection steps.

Active Publication Date: 2014-08-20
广东省科学院生物与医学工程研究所
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At present, there is no report on the detection method of plasticizers in sugar by high performance liquid chromatography tandem mass spectrometry

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  • High performance liquid chromatography-tandem mass spectrometry detection method of plasticizer in sugar
  • High performance liquid chromatography-tandem mass spectrometry detection method of plasticizer in sugar
  • High performance liquid chromatography-tandem mass spectrometry detection method of plasticizer in sugar

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specific Embodiment approach 1

[0086] Specific implementation mode 1: Addition recovery experiment in white granulated sugar

[0087] Take a white granulated sugar sample and process it according to the above-mentioned experimental steps, inject the sample to detect the plasticizer content of the sample, and the results are as follows: image 3 As shown, the results show that except for DEHP, which has a weak peak shape, other plasticizers have not been detected. Substituting into the standard curve for calculation, the detection result of DEHP is lower than the detection limit range, showing that it has not been detected.

[0088] On this basis, we conducted the spike recovery experiment of 16 kinds of plasticizers in white sugar, the spiked values ​​were 0.05 mg / L, 0.1 mg / L and 0.5 mg / L, and 6 a parallel experiment. Experimental results such as Figure 4 (0.1 mg / kg spiked), as shown in Table 4, at the three spiked levels, the spiked recoveries ranged from 81.6% to 110%, and the standard deviations of th...

specific Embodiment approach 2

[0092] Specific embodiment 2: the detection of plasticizer in rock sugar

[0093] After taking a sample of rock sugar and pulverizing it into powder, it was processed according to the above-mentioned experimental procedures, and the plasticizer content of the sample was detected by sampling. The results were as follows: Figure 5 As shown, the detection result is the detection of DEHP, and the detection value is 0.095 mg / L. Substituting it into the formula (1) to calculate the DEHP content in the rock sugar sample is 0.238 mg / kg. The results show that there is a small amount of DEHP residue in rock sugar. The reason may be that the rock sugar production process is the redissolution and crystallization of white sugar, which is more complicated than white sugar, and the possibility of contact with plastic products increases, leading to the introduction of DEHP; or later Plastic packaging materials with high DEHP content are used in the packaging process, and the migration of pla...

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Abstract

The invention discloses a high performance liquid chromatography-tandem mass spectrometry detection method of a plasticizer in sugar, comprising the following steps: (1) preparing a standard solution and detecting by high performance liquid chromatography-tandem mass spectrometry to obtain retention time and standard spectrum diagram; (2) making relationship curves between concentration and chromatographic peak area according to varieties of phthalates from the standard spectrum diagram; (3) carrying out pretreatment of a sugar sample and detecting by high performance liquid chromatography-tandem mass spectrometry to obtain a sample spectrum diagram; and (4) comparing a detection result obtained from the step (3) with the standard curve obtained from the step (2), and calculating to determine the content of the plasticizer in sugar. The method provided by the invention has advantages of simple detection step and fast detection time. A simple and feasible detection method of a plasticizer can be provided for a food production enterprise or food inspection institution. Detection of the content of a plasticizer in sugar can be realized. In particular, high sensitivity detection of DINP can be realized.

Description

technical field [0001] The invention relates to a method for detecting plasticizers, in particular to a method for detecting plasticizers in sugar by high performance liquid chromatography tandem mass spectrometry. Background technique [0002] Plasticizers, also known as plasticizers, are widely used in industrial production to enhance the plasticity and flexibility of materials. The commonly used plasticizers are mainly Phthalate Acid Esters (PAEs for short). Plasticizers are widely used in various plastic products, and are easily migrated from various plastic products to the environment and even various foods. They are acutely toxic to the human body, cause hormone imbalance, and cause cancer, teratogenicity, and mutagenesis Harmful effects such as sex. Therefore, all countries in the world have strictly regulated the residues of phthalates in food. In my country, phthalates have been clearly defined as prohibited non-edible substances that are prohibited from being use...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 高裕锋甄振鹏郭剑雄李海乔余构彬
Owner 广东省科学院生物与医学工程研究所
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