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Method of determining residual quantity of methylmercury in aquatic products

A determination method and technology of methylmercury, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effects of stable derivative compounds, high extraction efficiency and high sensitivity

Inactive Publication Date: 2013-08-21
谱尼测试集团股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved in the present invention is to avoid the disadvantages of the above-mentioned prior art and propose a method for accurately qualitative and quantitative methylmercury residues in aquatic products by means of gas chromatography-mass spectrometry: the analysis method is derived Stable substance, good selectivity, hydrochloric acid, sodium chloride solution extraction, sodium tetraphenylborate derivatization method for GCMS determination, the pretreatment operation is simple and easy, no complicated enrichment treatment is required, after the sample is stripped and derivatized, The matrix is ​​simple, the background interference is small, and the instrument will not be polluted

Method used

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  • Method of determining residual quantity of methylmercury in aquatic products
  • Method of determining residual quantity of methylmercury in aquatic products
  • Method of determining residual quantity of methylmercury in aquatic products

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Embodiment 1

[0023] Using toluene as a solvent, prepare methylmercury series standard solutions according to Table 1, carry out pretreatment according to the above experimental conditions, and perform analysis and detection by gas chromatography-mass spectrometry. figure 1 is the total ion flow chromatogram of the detected methylmercury, figure 2 is the corresponding selective ion flow diagram, the ordinate in the two figures represents the ion intensity, and the abscissa represents the retention time, by figure 1 It is known that the peak eluting time of the target is appropriate, and the retention time is 5.198min. The peak area is plotted against the concentration, and according to the three parallel measurement results of each standard point, the standard curve of methylmercury is established, such as image 3 As shown, the ordinate in the standard curve graph represents the corresponding value of the ion peak area, and the abscissa represents the concentration. see image 3 The ob...

Embodiment 2

[0027] Accurately weigh 1 g of the prepared sample into a 50 ml centrifuge tube, add 5 mL of 6 mol / L hydrochloric acid solution, and ultrasonically extract for 30 min. After the extract is cooled, add 10mL of 10% sodium chloride aqueous solution, vortex for 3min, add 5ml of toluene, centrifuge at 4000r / min for 5min, transfer the toluene layer, repeat the 5ml toluene extraction twice, combine the toluene layer three times and use 5mL, Back extract the toluene layer with 1% L-cysteine ​​aqueous solution, transfer the extract to a 15ml centrifuge tube, add 1mL, 0.1% sulfuric acid solution to acidify (PH=3), 1ml saturated copper sulfate solution and 0.2mL, 0.1% four Derivatize with sodium phenyl borate solution, then add 1ml of n-hexane and shake for 30 minutes to extract, and analyze and detect with gas chromatography-mass spectrometry. Three parallel samples were made for this sample, and the test numbers were A, B, and C respectively. The analysis results are shown in Table 2, ...

Embodiment 3

[0033] The standard solution in the embodiment 1 is added in the aquatic product tissue treatment sample of the embodiment 2 at a fixed concentration, and the test is carried out according to the above-mentioned sample pretreatment process and instrument test conditions, and six additions are made to the sample, each The sample of standard-added content is repeatedly measured three times to get the average value, and according to the actual addition amount and the measured value, calculate the standard-added recovery rate of this sample, the experimental results are shown in Table 4, as can be seen from Table 4, the standard-added recovery rate of the sample is between 89.9%- 109% between.

[0034] Table 4 The recovery of standard addition of this sample

[0035] Amount added / ng 1 2 3 4 Actual measured average value / ng 50 100 200 500 Recovery rate,% 89.9 90.4 90.2 109

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Abstract

The invention relates to a method of determining a residual quantity of methylmercury in aquatic products. The method comprises mixedly extracting samples by a given volume of hydrochloric acid of a certain concentration and a sodium chloride solution, extracting with toluene, stripping with an L-cysteine ??solution, deriving with a given volume of derivative agents of two concentrations, pre-treating with n-hexane extraction, measuring the methylmercury by using a gas chromatography-mass spectrometry, wherein a temperature of an introduction port of the gas chromatography is set to be 250-300 DEG C, a carrying gas is set as a constant voltage mode, a nonpolar chromatographic column is selected and an interface temperature is 260-300 DEG C, passing the pre-treated sample through the gas chromatography and then into the chromatographic column, then heating, separating the sample in the chromatographic column, then entering into the mass spectrometry, determining nature of the sample according to a retention time of object compounds, characteristic ions and an abundance ratio, and determining an amount of the sample by an external-standard peak-area method. The method provided by the invention has advantages of accurate analysis method, good selectivity, high sensitivity and small interference.

Description

technical field [0001] The invention relates to a method for determining the residual amount of methylmercury in aquatic products, in particular to a method for determining the residual amount of methylmercury in aquatic products by using gas chromatography-mass spectrometry Background technique [0002] Methylmercury is an environmental pollutant with neurotoxicity. It mainly invades the central nervous system and can cause language and memory impairment. The main parts of its damage are the occipital lobe and cerebellum of the brain. Its neurotoxicity may be related to the disturbance of glutamine Acid reuptake and abnormal gene expression in nerve cells. Generally speaking, organic mercury is more toxic than inorganic mercury. Methylmercury is one of the most toxic mercury compounds in organic mercury. Due to its lipophilicity, bioaccumulation effect and Biomagnification effect, its toxicity is hundreds of times that of inorganic mercury. [0003] Inorganic mercury disch...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 宋薇
Owner 谱尼测试集团股份有限公司
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