UHPLC-MS/MS Determination of 13 Antibiotics in Water with Separation by Solid Phase Extraction
摘 要
采用固相萃取-超高效液相色谱-串联质谱法测定水中13种抗生素的含量。水样中的抗生素富集于PLS固相萃取柱上,用甲醇洗脱,洗脱液进行LC分离,以Endeavorsil C18色谱柱为分离柱,以不同体积比的0.4%(体积分数)甲酸-水溶液和甲醇-乙腈(40+60)溶液的混合液为流动相进行梯度洗脱。质谱分析中,采用电喷雾正离子源多反应监测模式检测。13种抗生素均在一定的质量浓度范围内与其对应的峰面积呈线性关系,方法的检出限(3S/N)在0.4~1.5 ng·L-1之间。以空白样品为基体进行加标回收试验,所得回收率在70.4%~101%之间,测定值的相对标准偏差(n=5)在1.1%~4.8%之间。
Abstract
UHPLC-MS/MS was applied to the determination of 13 antibiotics in water with solid phase extraction. The antibiotics in water sample were enriched on PLS solid phase extraction column, and then eluted with 5 mL of methanol. LC separation was performed by using Endeavorsil C18 chromatographic column as stationary phase, and the mixture of 0.4% (φ) formic acid solution and methanol-acetonitrile (40+60) solution with various ratios as mobile phase in gradient elution. ESI+ and multi-reaction monitoring were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 13 antibiotics were kept in definite ranges, with detection limits (3S/N) in the range of 0.4-1.5 ng·L-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 70.4%-101%, with RSD's (n=5) in the range of 1.1%-4.8%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201705010
所属栏目 工作简报
基金项目 国家自然科学基金青年科学基金(201506147)
收稿日期 2016/5/11
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备注陈小平(1960-),男,湖北武汉人,工程师,主要研究方向为仪器分析化学
引用该论文: CHEN Xiaoping,DENG Xiaojuan,LI Wenbin,GU Chunyan,JIN Lichuan. UHPLC-MS/MS Determination of 13 Antibiotics in Water with Separation by Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(5): 542~547
陈小平,邓小娟,李文斌,顾春燕,晋立川. 固相萃取-超高效液相色谱-串联质谱法测定水中13种抗生素的含量[J]. 理化检验-化学分册, 2017, 53(5): 542~547
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参考文献
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【2】WATKINSON A J, MURBY E J, KOLPIN D W, et al. The occurrence of antibiotics in an urban watershed:from wastewater to drinking water[J]. Sci Total Environ, 2009,407:2711-2723.
【3】DENG W J, LI N, ZHENG H L, et al. Occurrence and risk assessment of antibiotics in river water in Hong Kong[J]. Ecotoxicol Environ Saf, 2016,125:121-127.
【4】KUMMERER K. Antibiotics in the aquatic environment-a review part I[J]. Chemosphere, 2009,75:417-434.
【5】WANG H X, WANG N, WANG B, et al. Antibiotics in drinking water in shanghai and their contribution to antibiotic exposure of school children[J]. Environ Sci Technol, 2016,50:2692-2699.
【6】VOSOUGH M, RASHVAND M, ESFAHANI H M, et al. Direct analysis of six antibiotics in wastewater samples using rapid high-performance liquid chromatography coupled with diode array detector:a chemometric study towards green analytical chemistry[J]. Talanta, 2015,135:7-17.
【7】DU F Y, ZHEN X, SUN L, et al. Development and validation of polymerized high internal phase emulsion monoliths coupled with HPLC and fluorescence detection for the determination of trace tetracycline antibiotics in environmental water samples[J]. J Sep Sci, 2015,38(21):3774-3780.
【8】UDALOVA A Y, DMITRIENKO S G, NATCHUK S V, et al. Preconcentration of tetracycline antibiotics on a hyper-crosslinked polystyrene and their determination in waters by high-performance liquid chromatography[J]. J Anal Chem, 2015,70(3):292-297.
【9】周爱霞,苏小四,高松,等.高效液相色谱测定地下水、土壤及粪便中4种磺胺类抗生素[J].分析化学, 2014,42(3):397-402.
【10】金高娃,蔡友琼,于慧娟,等.超高效液相色谱法测定水产品中3种喹诺酮类药物残留量[J].理化检验-化学分册, 2012,48(1):43-45.
【11】宋战锋,朱婷婷,彭盛华.固相萃取富集-高效液相色谱-串联质谱法测定饮用水源水体中8种抗生素的残留量[J].理化检验-化学分册, 2015,51(1):66-72.
【12】邱盼子,郭欣妍,王娜,等.超高效液相色谱-串联质谱法同时测定制药废水中10种抗生素[J].色谱, 2015,33(7):722-729.
【13】ROSSMANN J, SCHUBERT S, GURKE R, et al. Simultaneous determination of most prescribed antibiotics in multiple urban wastewater by SPE-LC-MS/MS[J]. J Chromatogr B, 2014,969:162-170.
【14】闾幸,余卫娟,兰亚琼,等.固相萃取-液相色谱-串联质谱法测定猪栏废水中10种抗生素[J].理化检验-化学分册, 2014,50(3):273-277.
【15】ZHOU J L, KANG Y H. Matrix effect in high-performance liquid chromatography-tandem mass spectrometry analysis of antibiotics in environmental water samples[J]. J Sep Sci, 2013,36:564-571.
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