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Extraction and detection methods for mercury compounds in fish flesh

An extraction method and technology of mercury compounds, applied in the field of environmental analytical chemistry, can solve the problems of high toxicity of extraction reagents, high energy consumption, cumbersome extraction process, etc., and achieve the effect of simple and fast extraction method, simple extraction steps, and shortened operation time

Active Publication Date: 2017-03-15
TONGWEI +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because microwave extraction requires the process of heating and cooling, in practice, the overall extraction time is longer and consumes more energy; at the same time, this method uses a relatively high concentration (5mol / L) of hydrochloric acid in the extraction. It is easy to cause secondary pollution to the environment, and it is easy to cause health hazards to experimenters. On the other hand, low pH samples will also cause damage to subsequent analysis instruments.
[0006] Therefore, in the extraction of mercury compounds in fish meat, due to the problems of the existing technology that there are fewer types of mercury compounds extracted, the extraction process is cumbersome, the toxicity of the extraction reagents is high, the extraction time is long, and the efficiency is low, there is an urgent need for an efficient method. , fast, green extraction method

Method used

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  • Extraction and detection methods for mercury compounds in fish flesh
  • Extraction and detection methods for mercury compounds in fish flesh
  • Extraction and detection methods for mercury compounds in fish flesh

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment 1 extraction method and detection method of the present invention

[0044] (1) extraction method of the present invention

[0045] After the fresh crucian carp is dissected, take the fish meat on both sides, remove the fish bones, and put the fish meat in a meat grinder to grind the fish meat into meat sauce. Then put the sample into a vacuum freeze dryer, and freeze-dry it under vacuum at -45°C for 24 hours. Then put the dried sample into a pulverizer and pulverize it until it becomes powdery, and then use it as a fish sample.

[0046] Take 0.2g of the above fish sample in a 25mL conical centrifuge tube, add pH=4.0 (0.1molL -1 HCl to adjust the pH value), the concentration is 20mmolL -1Then put the sample in a vortex shaker and shake it at 3000rpm for 10min; after the extraction, put the sample in a centrifuge and centrifuge at 10000rpm for 5min; after centrifugation, take the supernatant , use a syringe filter to pass the sample through a 0.22 μm filter...

Embodiment 2

[0061] Screening of various process parameters in the extraction method of the present invention in embodiment 2

[0062] Referring to the method of Example 1, the following screening tests screened the types of thiol reagents, the amount of thiol reagents, different pH values ​​of thiol reagents and the parameters of the vortex.

[0063] 1. The effect of different sulfhydryl reagents on the extraction effect of methylmercury, ethylmercury and inorganic mercury in fish meat

[0064] The type of sulfhydryl reagent will affect the extraction effect of methylmercury, ethylmercury and inorganic mercury in fish meat. In order to screen out the best thiol reagents, the effects of three thiol reagents, 2-mercaptoethanol (2-ME), L-cysteine ​​(L-Cys), and dithizone (DTC), on the extraction recovery were investigated. Other process parameters: pH of the thiol reagent = 4.0; the dosage of the three thiol reagents is 20mmol / L, 5mL; the extraction shaking rate is 3000rpm, the time is 10mi...

Embodiment 4

[0083] Methodology Evaluation of Embodiment 4 The inventive method

[0084] 1. The specificity of the method

[0085] Utilize the method of the embodiment of the present invention 1, methylmercury, ethylmercury and inorganic mercury are detected in the freshwater fish and fish meat sold in the farmer's market in Chengdu, the supermarket, and the added amount is 0.2 μ g, and the spectrograms before and after the added standard are respectively as follows Figure 4 and Figure 5 as shown,

[0086] The results show that methylmercury, ethylmercury and inorganic mercury have obvious peak time intervals without interference from other impurities, which proves that the method of the present invention has good resolution, no interference from endogenous impurities, short peak time and rapid detection.

[0087] 2. Accuracy, reproducibility, detection limit and linear range of the method

[0088] Utilize the method of implementation 1 of the present invention to detect methylmercury...

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Abstract

The invention discloses an extraction method for mercury compounds in fish flesh. The extraction method comprises the following steps: preparing a fish flesh sample, adding a mercapto reagent for extraction, carrying out centrifugation, taking supernatant and carrying out filtering so as to obtain extract with enriched mercury compounds, wherein the mercapto reagent has a pH value of 3.0 to 8.0, optimally 4.0. According to the extraction method, the mercapto reagent is used as the only extraction reagent for extraction of mercury forms in the fish flesh sample; extraction steps are simple; the usage amount of the extraction reagent is low; and the method realizes simple high-efficiency low-toxicity extraction of mercury compounds in three forms, i.e., methyl mercury, ethyl mercury and inorganic mercury, from the fish flesh sample. The invention also discloses a detection method for the mercury compounds in fish flesh. The detection method needs no other operation and realizes analysis by directly injecting the obtained extract into a high performance liquid chromatography-cold vapor generation atomic fluorescence spectroscopy system; and the detection method can rapidly, accurately, stably and sensitively detect the mercury compounds in the three forms, and is applicable to promotion and application.

Description

technical field [0001] The invention belongs to the technical field of environmental analysis chemistry, in particular to a method for extracting and detecting mercury compounds in fish meat. Background technique [0002] Mercury is highly volatile and highly toxic, can cause harm to the health of the nervous system, and can accumulate in organisms. All countries have included mercury in the blacklist of priority pollutants. However, the toxicity, bioavailability, mobility and re-migration of mercury are closely related to its chemical form. Generally speaking, the toxicity of organic mercury is greater than that of inorganic mercury. Mercury and its compounds can be enriched in organisms and biomagnified through the food chain. Therefore, the accurate and efficient analysis of mercury species in fish is of great significance. [0003] For the speciation analysis of mercury in fish solid samples, pre-treatment has always been an important consideration. Extracting various...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 张凤枰冷庚焦宝玉饶瑾瑜李林高刘耀敏王殷洁
Owner TONGWEI
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