HUANG Si-jing,WANG Yi-jie,ZHU Bin,et al.Determination of Penicillin Residues in Water by Ultra High Performance Liquid Chromatography-High Resolution Mass Spectrometry[J].China Water & Wastewater,2021,37(2):112-116.
超高效液相色谱-高分辨质谱法测定水体中青霉素残留
- Title:
- Determination of Penicillin Residues in Water by Ultra High Performance Liquid Chromatography-High Resolution Mass Spectrometry
- 关键词:
- 青霉素; 固相萃取; 超高效液相色谱-高分辨质谱
- Keywords:
- penicillin; solidphase extraction; ultra high performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS)
- 摘要:
- 采用超高效液相色谱-高分辨质谱法(UPLC-HRMS)同时测定水体中7种青霉素残留。水样经Oasis HLB固相萃取小柱富集和净化后,用反向C18色谱柱分离,以0.1%的甲酸水溶液和乙腈溶液为流动相进行梯度洗脱,采用电喷雾离子源正离子模式进行检测。7种青霉素类化合物在1.0~20.0 μg/L的线性范围内,相关系数r均大于0.99,检出限为1~10 ng/L。实际水样加标回收率为91.15%~106.36%,相对标准偏差为2.30%~8.47%,均小于10%。该方法具有简单快速、准确度高等特点,可以实现水体中7种目标青霉素残留的测定。
- Abstract:
- High performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS) was used to determine 7 penicillin residues in water simultaneously. The water samples were enriched and purified by Oasis HLB solid phase extraction column and separated by reverse C18 chromatographic column. Then, gradient elution was implemented with 0.1% formic acid aqueous solution and acetonitrile solution as mobile phase. Finally, electrospray ion source positive ion mode was used for detection of penicillin. The correlation coefficient r of 7 penicillin compounds was greater than 0.99 and the detection limit was 1-10 ng/L in the linear range of 1.0-20.0 μg/L. Actual water sample with standard recovery rate was in the range of 91.15%-106.36%, and the relative standard deviations (RSDs) were 2.30%-8.47%, all less than 10%. The method was simple, fast and highly accurate, and could realize the determination of 7 target penicillin residues in water.
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