Method for determining seven indicative polychlorinated biphenyls in fish scales
A polychlorinated biphenyl and determination method technology, applied in the field of organic pollutants, can solve complex and cumbersome problems, cannot meet the detection requirements of large batches of samples, and has not been reported, so as to improve purification efficiency, meet daily use requirements, and improve the extraction effect. Enhanced effect
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Embodiment 1
[0064] The present embodiment comprises the following contents to the test of seven polychlorinated biphenyls in grass carp fish scales:
[0065] The collected 6 batches of grass carp scales were freeze-dried and pulverized evenly. Weighed 2g samples into a 50mL Teflon tube, added 50μL (1000ng / mL) PCB198 as an internal standard, and used 5mL HNO 3 :H 2 o 2 (1:1, V:V) mixed solution digested hard fish scales at 60°C, added ultrapure water, and accelerated solvent extraction with 10mL n-hexane-ethyl acetate (1:1, volume ratio) (temperature 50°C, pressure 1800psi, time 18min), purified with concentrated sulfuric acid (95%, mass percentage), then purified with 9g of basic alumina-magnesia-anhydrous sodium sulfate (5:2:1) mixed particles, centrifuged, and transferred the extract Put it in a heart-shaped bottle, concentrate it by rotary evaporation, make it up to 1mL with nonane, detect it by gas chromatography-electron capture detector (ECD), and quantify it by internal standard ...
Embodiment 2
[0093] The present invention comprises the following contents to the test of seven polychlorinated biphenyls in carp fish scales:
[0094] The collected 6 batches of carp scales were freeze-dried and pulverized evenly. Weighed 2g samples into a 50mL Teflon tube, added 50μL (1000ng / mL) PCB198 as an internal standard, and added 5mL HNO 3 :H 2 o 2 (1:1, V:V) mixed solution digested hard fish scales at 60°C, added ultrapure water, and accelerated solvent extraction with 10mL n-hexane-ethyl acetate (1:1, volume ratio) (temperature 50°C, pressure 1800psi, time 18min), purified with concentrated sulfuric acid (95%, mass percentage), then purified with 9g of basic alumina-magnesia-anhydrous sodium sulfate (5:2:1) mixed particles, centrifuged, and transferred the extract Put it in a heart-shaped bottle, concentrate it by rotary evaporation, make it up to 1mL with nonane, detect it by gas chromatography-electron capture detector (ECD), and quantify it by internal standard method.
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Embodiment 3
[0102] The collected 6 batches of tilapia fish scales were tested according to the pretreatment method and instrument conditions of Example 1, and the test results are shown in Table 4:
[0103] Table 4 Test results of seven PCBs in tilapia fish scales
[0104]
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