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Method for detecting methyl mercury, ethyl mercury and inorganic mercury in aquatic feed

A technology for aquatic feed and methylmercury, applied in the detection of methylmercury in aquatic feed, simultaneous extraction and detection of methylmercury, ethylmercury and inorganic mercury, can solve the health hazards of experimenters, unpredictable detection results, separation cumbersome conditions and other problems, to achieve the effect of reducing the mass transfer distance, high accuracy, and simple extraction process

Active Publication Date: 2015-12-30
四川威尔检测技术股份有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] (1) Aquafeeds are mainly in solid form. The above method is suitable for the content detection of mercury forms in liquid samples. If it is used to detect the content of mercury forms in solid form aquatic feed, the detection effect is unpredictable;
[0005] (2) The above method is to separate the constant mercury form in the water sample under the cooperation of L-cysteine, ammonia water and ammonium acetate. The separation conditions are complicated and time-consuming, and the ammonia water and ammonium acetate used in the separation belong to Toxic reagents will not only cause health hazards to experimenters, but also easily cause secondary pollution to the environment

Method used

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  • Method for detecting methyl mercury, ethyl mercury and inorganic mercury in aquatic feed
  • Method for detecting methyl mercury, ethyl mercury and inorganic mercury in aquatic feed
  • Method for detecting methyl mercury, ethyl mercury and inorganic mercury in aquatic feed

Examples

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Embodiment 1

[0040] This embodiment proposes a method for detecting methylmercury, ethylmercury and inorganic mercury in aquatic feed, comprising the following steps:

[0041] A, take the aquatic feed sample and make it into powder after drying, add L-cysteine, after shaking and centrifuging, extract the supernatant and filter to prepare the sample to be tested;

[0042] B. After preparing the sample to be tested with L-cysteine ​​into a test solution with a concentration of 10 μg / L, use high-performance liquid chromatography-cold vapor generation atomic fluorescence spectrometer for detection, and the detection conditions meet:

[0043] Mobile phase: a mixed solution composed of 5% (v / v) acetonitrile, 60mmol / L ammonium acetate and 10mmol / LL-cysteine,

[0044] Flow rate: 0.8mL / min, injection volume: 80μL,

[0045] Lamp current: 25mA, multiplier tube negative high voltage: 250mA,

[0046] Carrier gas: Ar,

[0047] Oxidant: K with a mass volume ratio of 1% 2 S 2 o 8 and 3% NaOH,

[0048...

Embodiment 2

[0051] The method for the detection of methylmercury, ethylmercury and inorganic mercury in the aquatic feed involved in the present embodiment comprises the following steps:

[0052] A, take the aquatic feed sample and make it into powder after drying, add L-cysteine, after shaking and centrifuging, extract the supernatant and filter to prepare the sample to be tested;

[0053] B. After preparing the sample to be tested with L-cysteine ​​into a test solution with a concentration of 10 μg / L, use high-performance liquid chromatography-cold vapor generation atomic fluorescence spectrometer for detection, and the detection conditions meet:

[0054] Mobile phase: a mixed solution composed of 5% (v / v) acetonitrile, 60mmol / L ammonium acetate and 10mmol / LL-cysteine,

[0055] Flow rate: 1.2mL / min, injection volume: 120μL,

[0056] Lamp current: 35mA, multiplier tube negative high voltage: 300mA,

[0057] Carrier gas: Ar,

[0058] Oxidant: K with a mass volume ratio of 3% 2 S 2 o ...

Embodiment 3

[0062] The difference between this example and Example 1 is that in step A involved in this example, the aquatic feed sample is dried at 55° C. for 20 hours, and then powdered by a pulverizer.

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Abstract

The invention discloses a method for detecting methyl mercury, ethyl mercury and inorganic mercury in aquatic feed. The method comprises the following steps: drying an aquatic feed sample and preparing the sample into powder; adding L-cysteine; after vibrating and centrifuging, extracting supernatant liquid and filtering to prepare a sample to be detected; preparing the sample to be detected into a solution to be detected with the concentration of 10 micrograms / L by using the L-cysteine, and detecting by using a high performance liquid chromatography-cold steam generation atom fluorescence spectrophotometer. According to the method disclosed by the invention, the L-cysteine is used as an only extracting agent for mercury forms in the aquatic feed; the various forms of the mercury can be simply, rapidly and reliably extracted from the aquatic feed with a complicated base body by adopting a vibration and separation extraction form; after the extraction is finished, extra operations are not needed and an extracting solution is directly injected into the high performance liquid chromatography-cold steam generation atom fluorescence spectrophotometer to be analyzed; compared with reported methods, the method is simple and rapid, reagents are green and toxin-free, and the method is accurate and sensitive and has low detection limit.

Description

technical field [0001] The invention is a method for detecting methylmercury, ethylmercury and inorganic mercury in aquatic feed, specifically relates to a method for simultaneously extracting and detecting methylmercury, ethylmercury and inorganic mercury from aquatic feed, and belongs to the detection of heavy metal mercury technology field. 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. Aquafeed is the main source of nutrients in aquaculture. The mercury and its compounds contained in it can be enriched in organisms and biomagnified through the food chain. my country is the...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N21/64G01N1/28
Inventor 张凤枰冷庚刘耀敏焦宝玉李林高饶瑾瑜王殷洁
Owner 四川威尔检测技术股份有限公司
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