Method for measuring residual quantity of diethylstilbestrol in aquatic products by utilizing liquid chromatogram fluorescent method

Abstract

The invention discloses a method for measuring residual quantity of diethylstilbestrol in aquatic products by utilizing a liquid chromatogram fluorescent method, comprising the following steps: (1) weighing 100g of ground aquatic product samples in a 50mL plastic centrifuge tube, adding 20mL of acetic ether, homogenizing for 230s, centrifuging for 10min with the speed of 7000r / min, moving the acetic ether layer to a 100mL pear-shaped flask, utilizing 2mL of normal hexane and acetic ether with a volume ratio of 85:15 to dissolve residue, and then stirring for 6min; (2) activating an SLH column by utilizing 5mL of normal hexane and 5mL of acetic ether, adding extracting solution on the SLH column, utilizing 10mL of normal hexane and acetic ether with the volume ratio of 82:20 to elute by controlling the flow rate at 2mL / min, collecting eluent, carrying water bath at the temperature of 450 DEG C, and then carrying out nitrogen drying till the original state; and (3) adding 1mL of sulfuric acid to the centrifuge tube of nitrogen drying, then adding 8mL of water in the centrifuge tube, utilizing 1mL of mobile phase for metering volume so as to be measured by an efficient liquid phase chromatogram. The method for measuring residual quantity of diethylstilbestrol in aquatic products has advantages of low cost, simple method, and low measuring limit, is suitable for popularization and use in the production and practice and is a technology demanded by the market, and has positive social meaning and social demand.

Description

technical field

[0001] A method for determining the residual amount of diethylstilbestrol in aquatic products by using liquid chromatography fluorescence method. Background technique

[0002] Diethylstilbestrol is a hormonal drug, which can promote the growth of fish and other living organisms when added to feed, and is currently widely used in aquaculture.

[0003] As a synthetic chemical substance, diethylstilbestrol has strong estrogen-like effects. It has been confirmed by scientific experiments that diethylstilbestrol is a carcinogen, and long-term consumption will cause harm to human and animal health, even cause cancer, and even threaten life. Most countries in the world have banned the use of diethylstilbestrol in feed. Announcement No. 193 of the Ministry of Agriculture of my country stipulates that as of May 15, 2002, the use of diethylstilbestrol and its salt and ester preparations in all food animals shall be stopped.

[0004] In order to meet the requirements...

Examples

Embodiment

[0024] Take the determination of diethylstilbestrol residues in sea cucumbers as an example:

[0025] (1) Weigh 10g of minced aquatic product samples into a 50ml plastic centrifuge tube, add 20ml of ethyl acetate, homogenize for 30s, centrifuge at 7000r / min for 10min, pipette the ethyl acetate layer into a 100ml pear-shaped bottle, and remove the residue Add 10ml of ethyl acetate, repeat the extraction once, combine the ethyl acetate layer after centrifugation, evaporate to dryness at 45°C, and dissolve the residue with 2ml of n-hexane:ethyl acetate with a volume ratio of 85:15, and stir for 6 minutes;

[0026] (2) Activate the SLH column with 5ml n-hexane and 5ml ethyl acetate, add the extract to the SLH column, and control the flow rate to 2ml / min; use 2ml n-hexane, 2ml volume ratio of 85:15 n-hexane:acetic acid Rinse the SLH column with ethyl ester mixed solution, elute with 10ml of n-hexane:ethyl acetate mixed solution with a volume ratio of 82:20, control the flow rate at...

technical field

[0001] A method for determining the residual amount of diethylstilbestrol in aquatic products by using liquid chromatography fluorescence method. Background technique

[0002] Diethylstilbestrol is a hormonal drug, which can promote the growth of fish and other living organisms when added to feed, and is currently widely used in aquaculture.

[0003] As a synthetic chemical substance, diethylstilbestrol has strong estrogen-like effects. It has been confirmed by scientific experiments that diethylstilbestrol is a carcinogen, and long-term consumption will cause harm to human and animal health, even cause cancer, and even threaten life. Most countries in the world have banned the use of diethylstilbestrol in feed. Announcement No. 193 of the Ministry of Agriculture of my country stipulates that as of May 15, 2002, the use of diethylstilbestrol and its salt and ester preparations in all food animals shall be stopped.

[0004] In order to meet the requirements...

Examples

Embodiment

[0024] Take the determination of diethylstilbestrol residues in sea cucumbers as an example:

[0025] (1) Weigh 10g of minced aquatic product samples into a 50ml plastic centrifuge tube, add 20ml of ethyl acetate, homogenize for 30s, centrifuge at 7000r / min for 10min, pipette the ethyl acetate layer into a 100ml pear-shaped bottle, and remove the residue Add 10ml of ethyl acetate, repeat the extraction once, combine the ethyl acetate layer after centrifugation, evaporate to dryness at 45°C, and dissolve the residue with 2ml of n-hexane:ethyl acetate with a volume ratio of 85:15, and stir for 6 minutes;

[0026] (2) Activate the SLH column with 5ml n-hexane and 5ml ethyl acetate, add the extract to the SLH column, and control the flow rate to 2ml / min; use 2ml n-hexane, 2ml volume ratio of 85:15 n-hexane:acetic acid Rinse the SLH column with ethyl ester mixed solution, elute with 10ml of n-hexane:ethyl acetate mixed solution with a volume ratio of 82:20, control the flow rate at...