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| Determination of 13 Sulfonamide Residues in Water by Ultrasound assisted Dispersive Liquid-Liquid Microextraction Coupled with Ultra Performance Liquid Chromatography-Tandem Quadrupole Mass Spectrometry |
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| DOI： |
| KeyWord:ultrasonic assisted dispersive liquid-liquid microextraction(UA-DLLME) ultra performance liquid chromatography coupled with tandem quadrupole mass spectrometry(UPLC-MS/MS) sulfonamide water |
| Author | Institution |
| LI Xiao-jing，YU Hong，YANG Rong，GAN Ping-sheng，LIU Miao，LI Zhi-feng |
广州市疾病预防控制中心 |
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| Abstract: |
| A simple and rapid method was established for the preconcentration and determination of 13 sulfonamide residues in water samples by ultrasonic-assisted dispersive liquid-liquid microextraction(UA-DLLME) coupled with ultra performance liquid chromatography-tandem quadrupole mass spectrometry(UPLC-MS/MS)．The target compounds in water samples were synergistically extracted in ultrasonic dispersed mode and separated on a C18(100 mm×2.1 mm,1.7 μm) column with acetonitrile-0.1% formic acid solution as mobile phase，and determined by UPLC-MS/MS under multiple reactions monitoring(MRM) mode．The kind and dosage of extraction agent and dispersing agent，extraction time，dosage of sodium chloride and pH conditions were optimized．Under the optimized conditions，the calibration curves of 13 sulfonamides were linear in the certain concentration range with correlation coefficients greater than 0.998.The detection limits of the method(S/N＝3) were between 0.6 ng/L and 2.4 ng/L.The average recoveries of sulfonamides at three spiked levels in water sample ranged from 80.3%to 101.8%with relative standard deviations(RSD，n＝5) of 0.7%-4.5%.The developed method was simple，environment-friendly and sensitive,and was suitable for the determination of multiple sulfonamide residues in water. |
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