Naing Nyi Nyi, Li Sam Fong Yau, Lee Hian Kee
Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore; National University of Singapore Environmental Research Institute, T-Lab #02-01, 5A Engineering Drive 1, Singapore 117411, Singapore.
Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore; National University of Singapore Environmental Research Institute, T-Lab #02-01, 5A Engineering Drive 1, Singapore 117411, Singapore.
J Chromatogr A. 2016 Jan 4;1427:29-36. doi: 10.1016/j.chroma.2015.12.012. Epub 2015 Dec 8.
A facile method of extraction using porous membrane protected micro-solid phase extraction (μ-SPE) with a graphene-based sorbent followed by high performance liquid chromatography-ultraviolet detector was developed. The reduced graphene oxide (r-GO) (1mg), synthesized from graphite oxide, was enclosed in a polypropylene bag representing the μ-SPE device, which was used for the extraction of estrogens such as estrone, 17β-estradiol, 17α-ethynylestradiol and diethylstilbestrol in water. The r-GO obtained was identified and characterized by Fourier transform infrared, transmission electron microscopy, scanning electron microscopy and thermogravimetric analysis. The sorbent was loaded with sodium dodecyl sulfate by sonication to prevent agglomeration in aqueous solution. With this method, low limits of detection of between 0.24 and 0.52 ng L(-1) were achieved. For estrogen analysis a linear calibration range of 0.01-100 μg L(-1) was obtained, with the coefficients of determination (r(2)) higher than 0.992. This proposed method was successfully applied to determine estrogens in water.
开发了一种简便的萃取方法，该方法采用多孔膜保护的微固相萃取（μ-SPE），结合基于石墨烯的吸附剂，随后进行高效液相色谱-紫外检测。由氧化石墨合成的还原氧化石墨烯（r-GO）（1mg）被封装在一个聚丙烯袋中，构成μ-SPE装置，用于萃取水中的雌激素，如雌酮、17β-雌二醇、17α-乙炔基雌二醇和己烯雌酚。通过傅里叶变换红外光谱、透射电子显微镜、扫描电子显微镜和热重分析对所得的r-GO进行了鉴定和表征。通过超声处理将十二烷基硫酸钠负载到吸附剂上，以防止其在水溶液中团聚。采用该方法，检测限低至0.24至0.52 ng L⁻¹。对于雌激素分析，获得了0.01 - 100 μg L⁻¹的线性校准范围，测定系数（r²）高于0.992。该方法成功应用于水中雌激素的测定。
