Pretreatment method for ultrasonic extraction of multiple antibiotics in sediment

A sediment and antibiotic technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high price of accelerated solvent extraction instrument and extraction pool, high experimental threshold, cumbersome steps, etc., to overcome poor stability and adapt to Wide range of effects and simple methods

Inactive Publication Date: 2018-02-13
CHINESE RES ACAD OF ENVIRONMENTAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The experimental threshold of accelerated solvent extraction (ASE) is high, and the price of accelerated solvent extraction instrument and extraction cell is high; Soxhlet extraction takes a long time and the steps are cumbersome; microwave-assisted extraction takes a long time to process samples and requires Consume more manpower

Method used

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  • Pretreatment method for ultrasonic extraction of multiple antibiotics in sediment
  • Pretreatment method for ultrasonic extraction of multiple antibiotics in sediment
  • Pretreatment method for ultrasonic extraction of multiple antibiotics in sediment

Examples

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Embodiment 1

[0029] Embodiment 1: A kind of pretreatment method of multiple antibiotics in ultrasonic extraction sediment

[0030] See attached Figure 1~4 As shown, weigh 2g of diatomaceous earth, put it into a 30mL glass centrifuge tube, add 20ul internal standard mixture (ciprofloxacin-D 8 , Sulfamethoxazole-D 4 , trimethoprim- 13 C 3 , Demethyltetracycline, Sulfadiazine- 13 C 6 )overnight. Then prepare extractant, described extractant can be the mixed solution of the acetonitrile of volume ratio 1:1 and EDTA-McIIvaine or citric acid buffer, extractant 30mL, ultrasonic 15min, extraction frequency is 3 times, rotary evaporation temperature 40 ℃ .

[0031] Use 10mL methanol and 10mL ultrapure water to activate the SAX and HLB small columns under the action of gravity in turn, connect the two small columns in series with the modified connector, after the water sample passes through the column, use 10mL ultrapure water and 10mlL1-5% methanol Rinse the small column with aqueous solut...

Embodiment 2

[0034] Embodiment 2: A kind of pretreatment method of multiple antibiotics in ultrasonic extraction sediment

[0035] Weigh 2g of diatomaceous earth, put it into a 30mL glass centrifuge tube, add 20µL internal standard mixture (ciprofloxacin-D 8 , Sulfamethoxazole-D 4 , trimethoprim- 13 C 3 , Demethyltetracycline, Sulfadiazine- 13 C 6 )overnight. Then prepare the extractant, the extractant can be a mixture of acetonitrile and EDTA-McIIvaine with a volume ratio of 1:1, extract 30ml, vortex, ultrasonic for 15min, the number of extractions is 3 times, and the rotary evaporation temperature is 40°C.

[0036] Use 10mL methanol and 10mL ultrapure water to activate the HLB column under the action of gravity in turn. After the water sample passes through the column, rinse the column with 10mL ultrapure water and 10mlL1-5% methanol aqueous solution, and then put the solid phase extraction column in Vacuum for 2 hours to dryness, then elute with 6mL methanol and 6mL methanol conta...

Embodiment 3

[0038] Embodiment 3: A kind of pretreatment method of multiple antibiotics in ultrasonic extraction sediment

[0039] Weigh 2g of diatomaceous earth, put it into a 30mL glass centrifuge tube, add 20µL internal standard mixture (ciprofloxacin-D 8 , Sulfamethoxazole-D 4 , trimethoprim- 13 C 3 , Demethyltetracycline, Sulfadiazine- 13 C 6 )overnight. Then prepare the extractant, the extractant can be a mixture of acetonitrile and EDTA-McIIvaine with a volume ratio of 1:1, extract 30mL, vortex, ultrasonic for 30min, the number of extractions is 3 times, and the rotary evaporation temperature is 40°C.

[0040] Use 10mL methanol and 10mL ultrapure water to activate the SAX and HLB small columns under the action of gravity in turn, connect the two small columns in series with the modified connector, after the water sample passes through the column, use 10mL ultrapure water and 10mL 5% methanol aqueous solution Rinse the small column, and then pump the solid phase extraction colu...

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Abstract

The invention discloses a pretreatment method for the ultrasonic extraction of multiple antibiotics in a sediment. The pretreatment method comprises the following steps: 1, freeze-drying the sedimentor sandy soil, pulverizing, and screening by a 200-mesh sieve to obtain a sample; 2, putting the sample obtained in the step 1 and an internal standard liquid in a centrifuge tube; 3, adding an extraction agent into the centrifuge tube, conducting ultrasonic treatment for 15-30 minutes, then centrifuging, obtaining a liquid supernatant, and repeating for at least twice; 4, evaporating the liquid supernatant obtained in the step 3 until the volume no longer changes, then redissolving with ultrapure water to 300 mL, and regulating the pH to 2-9 to obtain a water sample; and 5, extracting the sample. The pretreatment method is relatively low in cost, and overcomes the defects of loss of the antibiotics caused by relatively poor stability of the antibiotics and relatively high temperature in the accelerated solvent extraction process.

Description

technical field [0001] The invention belongs to the field of residual detection of trace organic pollutants in sediment environment, and in particular relates to a pretreatment method for ultrasonic extraction of various antibiotics in sediment. Background technique [0002] According to the "China's First National Antibiotic Usage and Discharge Inventory" issued by the Chinese Academy of Sciences, in 2013 China's antibiotic production was 248,000 tons, and the consumption was 162,000 tons, of which 52% were for animals and 48% were for humans. , More than 50,000 tons of antibiotics are discharged into the water and soil environment a year. my country's Pearl River, Yellow River, Yangtze River, Haihe River, Taihu Lake, etc. have been detected to varying degrees, and the content of some antibiotics is at a relatively high level, reaching thousands of ng·L-1. Sediment, as an important "sink" of pollutants in the water environment and an internal load that is difficult to redu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 刘晓晖卢少勇吴亦潇郭睿孟伟郑丙辉张维昊毕斌
Owner CHINESE RES ACAD OF ENVIRONMENTAL SCI
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