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离线固相萃取用于环境水中药物和个人护理产品的预浓缩及其反相高效液相色谱法同时测定。

Offline solid-phase extraction for preconcentration of pharmaceuticals and personal care products in environmental water and their simultaneous determination using the reversed phase high-performance liquid chromatography method.

作者信息

Dhodapkar Rita, Kumar Anupama

机构信息

Chemistry Department, Visvesvaraya National Institute of Technology, Nagpur, 440010, India.

Waste water Technology Division, National Environmental Engineering Research Institute (CSIR), Nagpur, 440020, India.

出版信息

Environ Monit Assess. 2016 Sep;188(9):512. doi: 10.1007/s10661-016-5510-1. Epub 2016 Aug 9.

Abstract

The present study reports a precise and simple offline solid-phase extraction (SPE) coupled with reversed-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous determination of five representative and commonly present pharmaceuticals and personal care products (PPCPs), a new class of emerging pollutants in the aquatic environment. The target list of analytes including ciprofloxacin, acetaminophen, caffeine benzophenone and irgasan were separated by a simple HPLC method. The column used was a reversed-phase C18 column, and the mobile phase was 1 % acetic acid and methanol (20:80 v/v) under isocratic conditions, at a flow rate of 1 mL min(-1). The analytes were separated and detected within 15 min using the photodiode array detector (PDA). The linearity of the calibration curves were obtained with correlation coefficients 0.98-0.99.The limit of detection (LOD), limit of quantification (LOQ), precision, accuracy and ruggedness demonstrated the reproducibility, specificity and sensitivity of the developed method. Prior to the analysis, the SPE was performed using a C18 cartridge to preconcentrate the targeted analytes from the environmental water samples. The developed method was applied to evaluate and fingerprint PPCPs in sewage collected from a residential engineering college campus, polluted water bodies such as Nag river and Pili river and the influent and effluent samples from a sewage treatment plant (STP) situated at Nagpur city, in the peak summer season. This method is useful for estimation of pollutants present in microquantities in the surface water bodies and treated sewage as compared to nanolevel pollutants detected by mass spectrometry (MS) detectors.

摘要

本研究报告了一种精确且简单的离线固相萃取(SPE)与反相高效液相色谱(RP-HPLC)联用的方法,用于同时测定五种具有代表性且普遍存在的药品及个人护理用品(PPCPs),这是一类新出现的水生环境污染物。通过简单的HPLC方法分离了包括环丙沙星、对乙酰氨基酚、咖啡因、二苯甲酮和三氯生在内的目标分析物列表。所用色谱柱为反相C18柱,流动相为1%乙酸和甲醇(20:80 v/v),在等度条件下,流速为1 mL min⁻¹。使用光电二极管阵列检测器(PDA)在15分钟内分离并检测分析物。校准曲线的线性相关系数为0.98 - 0.99。检测限(LOD)、定量限(LOQ)、精密度、准确度和耐用性证明了所开发方法的重现性、特异性和灵敏度。分析前,使用C18柱进行固相萃取,以预富集环境水样中的目标分析物。所开发的方法应用于评估和识别在夏季高峰期从一所住宅工程大学校园收集的污水、那格河和皮利河等受污染水体以及那格浦尔市一家污水处理厂(STP)的进水和出水样品中的PPCPs。与质谱(MS)检测器检测到的纳摩尔级污染物相比,该方法对于估算地表水体和处理后污水中微量存在的污染物很有用。

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