Method for measuring contents of various endocrine disrupters in estuarine sediments
A technology for endocrine disruptors and sediments, which is applied in measuring devices, soil material testing, material separation, etc., can solve problems such as insufficient response to endocrine disruptors, and achieves the effects of strong practicability, high detection accuracy, and loss reduction.
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Embodiment 1
[0030] see figure 1 , the present embodiment provides a method for measuring the content of various endocrine disruptors in estuarine sediments, comprising the following steps:
[0031] (1) Pretreatment of estuarine sediments: Weigh 5 g of freeze-dried estuary sediment samples, add ten kinds of target endocrine disruptor mixed standard solutions with a concentration of 100ug / L, add alumina and diatomaceous earth for grinding, wherein alumina : Diatomaceous earth: the mass ratio of freeze-dried estuary sediment is 1:1:9, the obtained solid particles are sieved, and an internal standard is added to complete the pretreatment;
[0032] (2) Soxhlet extraction: Take 1 mass part of the sample pretreated in step (1) and add it to a cellulose tube, add 40 mass parts of methanol / acetone (1:1, v / v) solution, and perform Soxhlet extraction for 8 hours , and then rotary evaporate the obtained extract to about 1-2 mL;
[0033] (3) Activation of the solid-phase cartridge: take a C18 solid-...
Embodiment 2
[0041] This embodiment provides a method for determining the content of various endocrine disruptors in estuary sediments, comprising the following steps:
[0042] (1) Sediment samples collected from an estuary in South China, freeze-dried estuary sediment samples, weighed 5g of freeze-dried estuary sediment samples, added ten kinds of target endocrine disruptor mixed standard solutions with a concentration of 100ug / L, and added oxidation Aluminum and diatomite are ground, wherein the mass ratio of aluminum oxide: diatomite: freeze-dried estuary sediment is 1:1.5:11, the obtained solid particles are sieved, and an internal standard is added to complete the pretreatment;
[0043] (2) Soxhlet extraction: Take 1 mass part of the sample pretreated in step (1) and add it to a cellulose tube, add 40 mass parts of methanol / acetone (1:1, v / v) solution, and perform Soxhlet extraction for 8 hours , and then rotary evaporate the obtained extract to about 1-2 mL;
[0044] (3) Activation ...
Embodiment 3
[0058] Embodiment 3: Soxhlet extraction time optimization
[0059] In order to make full and reasonable use of time and realize efficient extraction of various endocrine disruptors, the present invention optimizes the Soxhlet extraction efficiency, investigates the influence of different extraction times (4h, 6h, 8h and 10h) on the recovery rate, and the results are as follows: figure 2 shown. The experimental results show that with the increase of the Soxhlet extraction time, the recovery rate of the target endocrine disruptor increases continuously. When the extraction time is 8 hours, the increase rate of the recovery rate of each component slows down and basically tends to be constant. Therefore, the Soxhlet extraction time is selected as 8h, which not only ensures a higher recovery rate, but also saves time appropriately.
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