Detection method of content of estradiol in anaerobic granular sludge
An anaerobic granular sludge and detection method technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of difficult pretreatment and the existence of traces of estradiol, and achieve low detection limits, simple operation, and easy extraction The effect of low temperature
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Embodiment 1
[0037] (1) Sludge sample extraction
[0038] The collected sludge sample is subjected to freeze-drying treatment, using methanol as an extractant, using an ultrasonic instrument for ultrasonic extraction, diluting the extract with methanol / distilled water=1:20 (v / v), centrifuging (preferably centrifuging at 10000rpm for 10min ), collect the supernatant, repeat twice, and the gained supernatant is combined;
[0039] (2) Purification of supernatant
[0040] After the above supernatant was vacuum filtered, the Oasis HLB 3cc (60mg) solid phase extraction column (SPE column) of Waters Company was used to purify and enrich the estradiol therein, and ethyl acetate was used to remove the estradiol from the solid phase extraction column. After elution, add an internal standard, blow dry with nitrogen, and derivatize to obtain the test solution;
[0041] (3) Analysis of estradiol content by gas chromatography-tandem mass spectrometry
[0042] Utilize gas chromatography-tandem mass sp...
Embodiment 2
[0062] Anaerobic granular sludge in an upflow anaerobic sludge bed reactor for treating estrogen-containing wastewater was collected, and the collected sludge samples were freeze-dried for 48 hours with a freeze dryer. Put the mud sample in a glass sample bottle, use methanol as the extractant, use an ultrasonic instrument to ultrasonically extract at a frequency of 20kHz for 15min, dilute the extract with methanol / distilled water = 1:20 (v / v), and centrifuge at 10000rpm for 10min , collect the supernatant, repeat twice, and combine the supernatant. The supernatant after above-mentioned merging adopts Waters company Oasis HLB 3cc (60mg) solid-phase extraction column (SPE column) enrichment wherein estradiol after vacuum suction filtration, and solid-phase extraction column is washed with 5ml acetic acid successively before use Ethyl ester, 5ml methanol, and 10ml ultrapure water were passed through the column for activation. After enrichment, use 5ml 50% methanol to rinse the ...
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