Method for simultaneously detecting five medicaments in water
A detection method and water detection technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of non-negligible mixed toxicity and chronic toxicity effects, incomplete absorption and utilization of drugs, and low antibiotic content, etc., to achieve selectivity Strong, easy to handle, reproducible results
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Embodiment 1
[0053] Embodiment 1: recovery rate experimental result
[0054] Take 1000ml of ultrapure water in a brown glass bottle, add 1ml of 100μg / L mixed standard stock solution of 5 common drugs to each bottle of water sample, mix well and add a small amount of hydrochloric acid to adjust the pH of the water sample to about 3.0. Utilize 6mL chromatographically pure acetone, 6mL chromatographically pure methanol, 6mL 0.1% (m / v) formic acid aqueous solution containing 5mmol / L ammonium acetate, and 15-20mL ultrapure water to activate the HLB (500mg, 6cc) solid phase extraction column of Waters Company successively , control the flow rate to less than 1mL / min;
[0055] (2) Concentration and enrichment
[0056] After the enrichment is completed, dry the HLB solid-phase extraction column under nitrogen protection for 20 minutes, use 10mL of 5% ammonia water methanol solution to elute the HLB column, control the flow rate to less than 1mL / min, collect the eluate in a 10mL conical bottom gla...
Embodiment 2
[0063] Example 2: The recovery results of water samples from Beijing Olympic Park.
[0064] Take 1000ml of river water samples from Beijing Olympic Park in a brown glass bottle, and carry out the standard addition experiment according to the method in Example 1, while taking 1000ml of river water samples without adding standards, as a blank control.
[0065] The results of the spiked water samples were brought into the standard curve equation, and the concentrations of five common drugs in the water samples to be tested were finally obtained by calculation. The recovery rate was calculated, and the results are shown in Table 2.
Embodiment 3
[0066] Example 3: Measurement results of actual water samples in Wangyanggou, Shijiazhuang, Hebei.
[0067] 1000mL water samples from Ziyahe Wangyanggou (38°18′28″N, 114°24′45″E) were subjected to negative pressure suction filtration through a glass fiber membrane (Whatman, 0.45μm), and the filtrate was subjected to a 6mL chromatographic Pure acetone, 6mL chromatographically pure methanol, 6mL 0.1% (m / v) formic acid aqueous solution containing 5mmol / L ammonium acetate, 15-20mL ultrapure water activate the HLB cartridge, and control the flow rate at 2-5mL / min. Vacuum dry for 1 min after the enrichment, 10mL of 5% ammonia water methanol solution was used to elute the HLB column, the eluate was collected in a 10mL pointed-bottom glass colorimetric tube, and the eluate was slowly blown under nitrogen flow until it was nearly dry, and 400 μL of chromatographic pure The residue was dissolved in acetonitrile, vortexed, and tested.
[0068] The concentrations of five common drugs in ...
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