Key Laboratory of Urban Pollutant Conversion, Institute of Urban Environment, Chinese Academy of Sciences, Xiamen, China.
Nuclear Institute for Food and Agriculture, Tarnab, Peshawar, Pakistan.
Environ Toxicol Chem. 2019 Jul;38(7):1409-1422. doi: 10.1002/etc.4450. Epub 2019 Jun 21.
A quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based extraction and simultaneous dispersive solid-phase extraction (dSPE) clean-up method was developed for contaminants of emerging concern (CECs) in sediment samples. Hydration with a phosphate buffer (pH 2.0) and salting out with NaCl and MgSO facilitated the extraction and liquid-liquid portioning of the aqueous and organic phases. Cleanup of the extracts was achieved by florisil and C18 (1:1) sorbents in dSPE with minimal compromise of the analytes. The extracts were clean enough for determination by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The procedure was validated for preservatives, blood lipid regulators, analgesics and anti-inflammatory drugs, plasticizers, and other classes of CECs in sediment matrix spiked at 6 levels between 1- and 40-fold concentrations for CECs of varying analytical sensitivities. The recovery values were generally between approximately 27 and 120% and the relative standard deviation (%RSD) values were below 20% at 10- , 20- , and 40-fold spiking levels, albeit the recoveries for some analytes dropped at low spike concentrations. The method showed high sensitivity where the method detection limits (MDLs) were at low ppb levels for the majority of the analytes that ranged between 0.002 and 1.93 µg/kg. The method performance was also compared with well-established US Environmental Protection Agency (USEPA) Method 1694 by analyzing sediment samples collected from Yundang Lagoon (Xiamen, China) with field-incurred CEC residues. The sediment samples were detected with residues of parabens, gemfibrozil, ketoprofen, naproxen, fenoprofen, diclofenac, miconazole, carbamazepine, benzophenon-3, glibenclamide, sildinafil citrate, and some bisphenol analogues. Environ Toxicol Chem 2019;38:1409-1422. © 2019 SETAC.
建立了一种基于快速、简便、价廉、有效、耐用和安全（QuEChERS）的萃取方法，同时结合分散固相萃取（dSPE）净化，用于检测沉积物样品中的新兴污染物（CECs）。用磷酸缓冲液（pH 2.0）水合，用 NaCl 和 MgSO4 盐析，促进了水相和有机相的萃取和液液分配。通过 florisil 和 C18（1:1）在 dSPE 中的吸附剂进行萃取物的净化，对分析物的最小干扰下实现了净化。提取液干净到足以通过液相色谱-串联质谱法（LC-MS/MS）进行测定。该方法对防腐剂、血脂调节剂、镇痛药和抗炎药、增塑剂和其他类别的 CEC 进行了验证，在 6 个浓度水平（1-40 倍）下对不同分析灵敏度的 CEC 进行了测定。回收率一般在 27%到 120%之间，在 10-、20-和 40 倍加标水平下的相对标准偏差（%RSD）值低于 20%，尽管某些分析物在低加标浓度下回收率下降。该方法具有较高的灵敏度，大多数分析物的方法检测限（MDLs）处于低 ppb 水平，范围在 0.002 到 1.93µg/kg 之间。该方法还通过分析取自中国厦门云顶湖（Yundang Lagoon）的沉积物样品，与美国环保署（USEPA）方法 1694 进行了比较。沉积物样品中检测到了对羟基苯甲酸酯、吉非贝齐、酮洛芬、萘普生、芬布芬、双氯芬酸、咪康唑、卡马西平、二苯甲酮-3、格列本脲、西地那非枸橼酸盐和一些双酚类似物等 CEC 残留。Environ Toxicol Chem 2019;38:1409-1422. © 2019 SETAC.
