Huang Zhenzhen, Lee Hian Kee
Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore.
Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore; National University of Singapore Environmental Research Institute, T-Lab Building #02-01, 5A Engineering Drive 1, Singapore 117411, Singapore.
J Chromatogr A. 2015 Jul 3;1401:9-16. doi: 10.1016/j.chroma.2015.04.052. Epub 2015 May 7.
In this study, a metal-organic framework material, MIL-101, used as a micro-solid-phase extraction (μ-SPE) sorbent for efficient enrichment of five organochlorine pesticides (OCPs), including α-HCH, Aldrin, α-Chlordane, Dieldrin and p,p'-DDD from water samples, followed by gas chromatography-mass spectrometry, is reported. This study demonstrated a new application of MIL-101 using μ-SPE, an advantage of the latter being its ability to process complex aqueous matrices, due to the protection of the sorbent afforded by the hollow fiber membrane bag. Key factors affecting extraction efficiency were studied, including elution solvent, extraction and desorption time. Under the optimal extraction conditions, the calibration plots were linear from 0.05 to 50 ng/mL for α-HCH and p,p'-DDD, and 0.1 to 50 ng/mL for the other three analytes. The limits of detection were between 0.0025 and 0.016 ng/mL. The relative recoveries of the OCPs spiked into real water samples (at 5 ng/mL of each analyte) ranged from 87.6 to 98.6% with relative standard deviations of <10%.
本研究报道了一种金属有机骨架材料MIL-101，用作微固相萃取（μ-SPE）吸附剂，用于从水样中高效富集5种有机氯农药（OCPs），包括α-六氯环己烷、艾氏剂、α-氯丹、狄氏剂和p,p'-滴滴滴，随后进行气相色谱-质谱分析。本研究展示了MIL-101在μ-SPE中的新应用，后者的一个优点是能够处理复杂的水性基质，这是由于中空纤维膜袋对吸附剂的保护作用。研究了影响萃取效率的关键因素，包括洗脱溶剂、萃取和解吸时间。在最佳萃取条件下，α-六氯环己烷和p,p'-滴滴滴的校准曲线在0.05至50 ng/mL范围内呈线性，其他三种分析物在0.1至50 ng/mL范围内呈线性。检测限在0.0025至0.016 ng/mL之间。加标到实际水样中的OCPs（每种分析物浓度为5 ng/mL）的相对回收率在87.6%至98.6%之间，相对标准偏差<10%。
