Detecting method for trichlorfon enantiomers in culture pond bottom mud

A detection method, the technology of trichlorfon, applied in the field of detection of trichlorfon enantiomers in the bottom mud of breeding ponds, can solve the problems of undeveloped enantiomer levels

Inactive Publication Date: 2015-10-21
ZHEJIANG OCEAN UNIV
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Problems solved by technology

Existing literature has shown that there are differences in the toxicity of trichlorfon enantiomers, and the toxicity to AchE enzyme is (—)-trichlorfon>(+)-trichlorfon>racemic trichlorfon. In the study, trichlorfon has been analyzed as a single component, and no enantiomer level research has been carried out

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  • Detecting method for trichlorfon enantiomers in culture pond bottom mud
  • Detecting method for trichlorfon enantiomers in culture pond bottom mud
  • Detecting method for trichlorfon enantiomers in culture pond bottom mud

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Embodiment Construction

[0017] The present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments.

[0018] The detection method of trichlorfon chiral enantiomer in the culture pond bottom mud of the present embodiment comprises the following steps:

[0019] (1) Put 5g of sediment sample (dry weight) into a 50mL centrifuge tube, add 10g of anhydrous sodium sulfate to remove the moisture in the sample, add 1% acetic acid to acidify 20mL of acetonitrile, ultrasonically extract for 2min and centrifuge at 5000r / min for 5min , take the centrifuged upper layer extract, place it in a 250mL round-bottomed flask, repeat the above extraction steps twice, combine the three extracts for a total of 60ml, spin evaporate in a water bath at 27°C until concentrated to nearly 2-3mL, and the concentrated sample Add the solution to the CARB / NH2 solid-phase extraction column activated by 10ml acetonitrile in advance, rinse the round-bottomed flask with 7-8mL acet...

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Abstract

A detecting method for trichlorfon enantiomers in culture pond bottom mud includes the steps that a bottom mud sample is placed into a centrifugal tube, anhydrous sodium sulfate is added to remove water, acetic acid is added to acidize acetonitrile, centrifuging is performed after ultrasonic extraction is performed, an upper layer extracting solution is taken into a flask, the extracting process is repeated 2-3 times, extracting solutions are mixed, the mixed solution is subjected to rotary evaporation and concentration in a water bath at 27 DEG C, a concentrated solution is added into CARB / NH2 cartridges activated in advance, the acetonitrile is used for flushing the flask, flushing liquid passes through the CARB / NH2 cartridges, outflow liquid is collected, and the CARB / NH2 cartridges are blown through nitrogen to be almost dry, hexyl hydride / isopropanol is used for performing redissolving and volume constancy on the liquid to 1 mL, and then the liquid passes through a microporous filtering film of 0.22 micrometer to obtain a solution A; with the hexyl hydride / isopropanol being a moving phase, separation is performed on the trichlorfon enantiomers; a high-performance liquid chromatograph is used for detecting the solution A, (as shown in specifications) IC chiral columns are selected for usage, the temperature of the columns is 25 DEG C, the flow rate is 1 mL / min, and the wavelength is 207 nm. The trichlorfon chiral enantimoers can be successfully separated, in this way, the residual quantity of the trichlorfon enantiomers in the bottom mud is detected, and bases are provided for residual risk estimation and reasonable and safe using of trichlorfon in bottom mud culture.

Description

technical field [0001] The invention relates to a method for detecting the trichlorfon enantiomer in the bottom mud of a breeding pond. Background technique [0002] Trichlorfon [O,O-dimethyl-(2,2,2-trichloro-1-hydroxyethyl) phosphonate] belongs to chiral organophosphorus insecticides, which are commonly used in marine aquaculture or low Dosage of deworming and insecticide taken orally, trichlorfon is mainly used in seawater culture to kill copepods, rotifers, wild crustaceans, etc. in shrimp breeding, to prevent shrimp viruses carried by crustaceans from entering the culture pond It is an ideal drug for preventing viruses in clear ponds; it can kill wild small crabs, white shrimps, mole cricket shrimps and other harmful species in shrimp ponds and fish ponds that feed on shrimp fry or compete with shrimp fry for resources, so as to ensure the survival rate of shrimp fry and fry. [0003] At present, domestic and foreign studies have shown that in mariculture, the usual dos...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 欧阳小琨聂晶王阳光杨立业吴伟建郁迪高小峰王艳飞
Owner ZHEJIANG OCEAN UNIV
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