Method for detecting chloramphenicol, thiamphenicol, metronidazole residuals in prawns by using pressurized capillary electrochromatographic instrument

A technology of capillary electrochromatography and thiamphenicol, which is applied to instruments, measuring devices, scientific instruments, etc., can solve the problems of long analysis time, difficult to configure instruments, and low sensitivity of liquid chromatography, and achieves high sensitivity and detection cost. Low, low consumption effect

Active Publication Date: 2012-08-22
NINGBO ACAD OF SCI & TECH FOR INSPECTION & QUARANTINE
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The sensitivity of liquid chromatography is low, and the analysis time is long. Although the detection sensitivity and resolution of gas chromatogr

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  • Method for detecting chloramphenicol, thiamphenicol, metronidazole residuals in prawns by using pressurized capillary electrochromatographic instrument
  • Method for detecting chloramphenicol, thiamphenicol, metronidazole residuals in prawns by using pressurized capillary electrochromatographic instrument
  • Method for detecting chloramphenicol, thiamphenicol, metronidazole residuals in prawns by using pressurized capillary electrochromatographic instrument

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Embodiment Construction

[0022] The present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments.

[0023] A method for detecting chloramphenicol, thiamphenicol, and metronidazole residues in prawns by pressurized capillary electrochromatography, the steps are:

[0024] 1. Sample preparation: Cut the muscle tissue samples of prawns with their heads removed, cut them into pieces with scissors, homogenize them, and store them in a freezer;

[0025] 2. Sample pretreatment:

[0026] Thaw the sample, accurately weigh 2±0.01g (accurate to 0.01g) homogeneous sample and place it in a 50mL centrifuge tube, add 10mL of ethyl acetate, mix well with a vortex mixer for 5min, centrifuge at 4000r / min for 10min, collect For the supernatant, add 10 mL of ethyl acetate to the original centrifuge tube to repeat the extraction once, and combine the two supernatants. After adding 15 mL of n-hexane to degrease twice, the solution was rotary evaporated to drynes...

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Abstract

The invention relates to a method for detecting chloramphenicol, thiamphenicol, metronidazole residuals in prawns by using a pressurized capillary electrochromatographic instrument, which comprises the following steps of: preparing a sample; preparing standard chloramphenicol, thiamphenicol, metronidazole solutions; carrying out analysis on the solutions by using the pressurized capillary electrochromatographic instrument, namely, under the process conditions that a capillary electrochromatographic column taking phase reversal keys and C18 as packing is taken as a detecting column, a mobile phase is a mixed solution of a hydrogen diamine phosphate buffer solution (11-13 mmol/L, pH = 4-6) and acetonitrile, the volume ratio of the hydrogen diamine phosphate buffer solution to the acetonitrile is (90-70): (10-30), the applied voltage is minus 3-minus 5 kv, the pressure of the column is 9.6-9.8 MP, the temperature of the column is room temperature, the flow velocity of the mobile phase is 40- 60 mu L/min, and the sample size is 0.9-1.1 mu L, carrying out detection at a position (wavelength: 275 nm) by using an ultraviolet detector, and drawing standard curves; and after the sample is detected and analyzed, carrying out quantitative analysis on the sample according to the retention time of the sample, and carrying out quantitative analysis on the sample according to the peak area of the sample by using an external standard method. The method disclosed by the invention is efficient, accurate, less in organic reagent consumption, and high in sensitivity, and can satisfy the demands of daily detection on chloramphenicol, thiamphenicol, metronidazole drugs.

Description

technical field [0001] The invention belongs to the field of food safety-veterinary drug residues, in particular to a method for detecting residues of chloramphenicol, thiamphenicol and metronidazole in prawns by means of pressurized capillary electrochromatography. Background technique [0002] Chloramphenicol and thiamphenicol belong to the amide alcohol antibiotics and have broad-spectrum antibacterial ability. They are often used to prevent and control bacterial infectious diseases of fish and shrimp in aquaculture production; metronidazole is used to treat several kinds of trichomonas Infect. Chloramphenicol and thiamphenicol can inhibit the hematopoietic function of bone marrow and cause toxic and side effects such as aplastic anemia. Metronidazole can cause cancer and genetic mutations and other toxic and side effects. Many countries prohibit the use of them in animal feed and treatment, and stipulate that animal Chloramphenicol should not be detected in sexual food....

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Application Information

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IPC IPC(8): G01N30/88
Inventor 曹国洲肖道清朱晓艳刘在美杨文潮陈少鸿郑琳陈建国董洁莹
Owner NINGBO ACAD OF SCI & TECH FOR INSPECTION & QUARANTINE
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