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Method for testing methyl mercury and ethyl mercury in aquatic feed

A technology for aquatic feed and methylmercury, which is applied in the direction of measuring devices, material separation, and analytical materials, etc., can solve the problems that cannot fully meet the measurement requirements, and achieve the effects of low cost, high purging efficiency, high sensitivity and selectivity

Active Publication Date: 2019-01-11
INSPECTION AND QUARANTINE TECHNOLOGY CENTER ZHONGSHAN ENTRY EXIT INSPECTION AND QUARANTINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For aquafeeds with very low levels of methylmercury and ethylmercury, this method cannot fully meet the requirements for the determination of trace amounts of methylmercury and ethylmercury in aquafeeds

Method used

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  • Method for testing methyl mercury and ethyl mercury in aquatic feed
  • Method for testing methyl mercury and ethyl mercury in aquatic feed
  • Method for testing methyl mercury and ethyl mercury in aquatic feed

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Determination of methylmercury and ethylmercury in aquafeed samples involves the following steps:

[0054] a. Prepare sample solution and blank solution:

[0055] Dry the aquatic feed sample at 55-65°C for 24 hours to make a powder, weigh 1g of the powder, add 35-40mL of potassium bromide solution and 3mL of copper sulfate solution to mix to form a sample mixture, and place it in the sample bottle of the simultaneous distillation device After soaking for at least 2 hours, distill and extract simultaneously with 20-25 mL of dichloromethane placed in the solvent bottle of the simultaneous distillation device for at least 2 hours under water-cooling conditions, wherein the heating temperature of the sample mixture is 100-120 °C, and the heating temperature of dichloromethane 55-65°C, collect the organic phase, add 30-35mL deionized water and 3-4 polytetrafluoroethylene zeolites, heat at 60-65°C for stripping until the visible organic phase disappears, and then heat for 3-4...

Embodiment 2

[0125] According to the assay method described in Example 1, 14 batches of commercially available aquatic feed samples were tested, including 5 batches of fish feed, 2 batches of red fish meal for feed, 4 batches of shrimp feed and 3 batches of crab feed. The content of base mercury is shown in Table 9. It can be seen from Table 9 that methylmercury and ethylmercury may be contained in aquatic feed, and the content levels of methylmercury and ethylmercury are relatively low, but the detection limit and quantitative limit of the method of the present invention can meet the requirements of methylmercury in aquatic feed. Testing requirements for methylmercury and ethylmercury.

[0126] Table 9: Contents of methylmercury and ethylmercury in 14 batches of aquafeed samples

[0127]

[0128]

[0129] Note: "ND" means that the detection value of the analyte element is less than the quantitative limit of the method.

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Abstract

The invention discloses a method for testing the methyl mercury and the ethyl mercury in the aquatic feed. The method comprises the following steps of: using simultaneous distillation extraction method to simultaneously collect and extract samples, and water back extract; then performing a derivative reaction by using the sodium(tetra-n-propyl)borate as a derivatization reagent; finally, testing the methyl mercury and the ethyl mercury in the aquatic feed by using a full automatic alkyl mercury tester. According to the method for testing the methyl mercury and the ethyl mercury in the aquaticfeed, the method detection limit of the methyl mercury is 2mu / kg, the quantification limit is 6mu / kg, the relative standard deviation is 4.58%, and the average spike recovery is between 90.6% and 97.3%; the method detection limit of ethyl mercury is 4mu / kg, the quantification limit is 11mu / kg, the relative standard deviation is 5.19%, and the average recovery rate is between 89.2% and 96.7%. The sensitivity is high, the repeatability is good, the accuracy is good, and particularly the method detection limit and the quantitation limit are especially suitable for testing the methyl mercury and the ethyl mercury in the aquatic feed.

Description

【Technical field】 [0001] The invention relates to a method for measuring methylmercury and ethylmercury in aquatic feed, belonging to the technical field of detection methods. 【Background technique】 [0002] Mercury is a chemical substance with severe physiological toxicity. Its toxicity is closely related to its existing form. It mainly exists in the form of inorganic mercury and organic mercury in nature. The toxicity of organic mercury is stronger than that of inorganic mercury. Among them, methylmercury is the most toxic. Strong organic mercury, followed by ethyl mercury toxicity. Both methylmercury and ethylmercury have lipophilicity, bioaccumulation and biomagnification effects. They can be enriched in aquatic animals such as fish and shellfish, and are harmful to human health through migration and transformation through the food chain. The main target organ is the brain. Therefore, since the Minamata disease incident in Japan, the food-borne hazards caused by methylm...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 李浩洋汪海滨张宪臣郑传发何洁玲刘琼瑜李蓉
Owner INSPECTION AND QUARANTINE TECHNOLOGY CENTER ZHONGSHAN ENTRY EXIT INSPECTION AND QUARANTINE
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