陈海红,张聪璐,伦小文,孙志,梁宁,侯晓虹
CHEN Hai-hong,ZHANG Cong-lu,LUN Xiao-wen,SUN Zhi,LIANG Ning,HOU Xiao-hong(School of Pharmaceutical Engineering

• 1:沈阳药科大学制药工程学院

摘要(Abstract)：

目的建立专属、灵敏的固相萃取-液相色谱分析方法测定污水处理厂出水中6种残留药物(氯霉素、青霉素、水杨酸、泼尼松、尼莫地平、辛伐他汀)的质量浓度。方法样品经PEP固相萃取小柱预处理后,用HPLC法测定。色谱柱:C18柱(200 mm×4.6 mm,5μm);流动相:甲醇-体积分数0.2%乙酸水溶液,梯度洗脱;流速:1.0 mL.min-1;检测波长:230 nm。结果氯霉素、青霉素、水杨酸、泼尼松、尼莫地平、辛伐他汀质量浓度分别在0.2～20.0 mg.L-1、1.0～100.0 mg.L-1、0.1～10.0 mg.L-1、0.2～20.0 mg.L-1、0.1～10.0 mg.L-1、0.1～10.0 mg.L-1内线性关系良好,相关系数均大于0.999 3,精密度(RSD)为1.1%～1.9%,平均加样回收率在73.1%～100.2%内,样品溶液在12 h内稳定性良好。结论该方法简单、灵敏、准确,可用于水环境中残留药物的分析。
Objective To develop and validate a specific,sensitive and rapid method for the simultaneous determination of six pharmaceutical residues in aquatic environment by solid phase extraction-high performance liquid chromatography.The analytes included chloramphenicol,salicylic acid,penicillin,prednisone,nimodipine and simvastatin.Methods The sample pretreatment was operated on PEP solid phase extraction column.The analytes were separated and measured on a C18 column(200 mm×4.6 mm,5 μm)with gradient elution using methanol and 0.2% acetic acid in purified water at the flow rate of 1.0 mL · min-1,and the wavelength was set at 230 nm.Results The linear ranges of chloramphenicol,penicillin,salicylic acid,prednisone,nimodipine and simvastatin were 0.2-20.0,1.0-100.0,0.1-10.0,0.2-20.0,0.1-10.0,0.1-10.0 mg · L-1,respectively.The range of precision was 1.1%-1.9%.The average recoveries of the analytes were ranging from 73.1% to 100.2% for six analytes with relative standard deviation lower than 20.0%,and sample solutions were stable within 12 h.Conclusions The method is simple,sensitive,accurate and reliable for the determination of six target analytes in aquatic environment.

关键词(KeyWords)： 固相萃取;高效液相色谱法;水分析;残留药物
solid phase extraction;HPLC;water analysis;pharmaceutical residue

Abstract:

Keywords:

基金项目(Foundation): 中国博士后科学基金资助项目(2007001);; 沈阳市科技局大型仪器共享资助项目(090100)

作者(Author): 陈海红,张聪璐,伦小文,孙志,梁宁,侯晓虹
CHEN Hai-hong,ZHANG Cong-lu,LUN Xiao-wen,SUN Zhi,LIANG Ning,HOU Xiao-hong(School of Pharmaceutical Engineering

DOI: 10.14066/j.cnki.cn21-1349/r.2012.05.001

参考文献(References)：

• [1]DAUGHTON C G,TERNES T A.Pharmaceuticals andpersonal care products in the environment:agents ofsubtle change[J].Environ Health Perspect,1999,107:907-938.
• [2]陈新,伦小文,侯晓虹.水环境中药物污染分析的研究进展[J].沈阳药科大学学报,2010,27(2):157-162.
• [3]陈方荣,吴波,马培丽,等.固相萃取-液相色谱法同时检测4种酸性PPCPs[J].湖北大学学报:自然科学版,2011,33(2):168-173.
• [4]李利荣,吴宇峰,时庭锐,等.固相萃取技术在环境水质监测方法开发中的应用[J].环境科学与技术,2007,3:41-44.
• [5]ZHENG Qi-ye,WEINBERG H S.Trace analysis of tri-methoprim and sulfonamide,macrolide,quinolone,andtetracycline antibiotics in chlorinated drinking water u-sing liquid chromatography electrospray tandem massspectrometry[J].Anal Chem,2007,79:1135-1144.
• [6]谭建华,唐才明,余以义,等.高效液相色谱法同时分析城市河水中的多种抗生素[J].色谱,2007,25(4):546-549.
• [7]RENEW J E,HUANG C H.Simultaneous determinationof fluoroquinolone,sulfonamide,and trimethoprim anti-biotics in waste water using tandem solid phase extrac-tion and liquid chromatography-electrospray mass spec-trometry[J].Journal of Chromatography A,2004,1042:113-121.
• [8]徐维海.典型抗生素类药物在珠江三角洲水环境中的分布、行为与归宿[D].广州:中国科学院广州地球化学研究所,2007.
• [9]MARCHESE S,PERRET D,GENTILI A,et al.Deter-mination of non-steroidal anti-inflammatory drugs insurface water and wastewater by liquid chromatography-tandem mass spectrometry[J].Chromatogr,2003,58:263-269.
• [10]陈新,张聪璐,陈海红,等.固相萃取-液相色谱法测定水环境中4种非甾体抗炎药物[J].西北药学杂志,2010,25:323-325.
• [11]MIAO Xiu-sheng,METCALFE C D.Determination ofcholesterol-lowering statin drugs in aqueous samples u-sing liquid chromatography-electrospray ionization tan-dem mass spectrometry[J].Journal of ChromatographyA,2003,998:133-141.
• [12]GIRAND V G,MIEGE C,CHOUBERT J M,et al.Oc-currence and removal of estrogens and beta blockers byvarious processes in wastewater treatment plants[J].Science of the Total Environment,2010,408:4257-4269.