LEPABE - Laboratory for Process Engineering, Environment, Biotechnology and Energy, Faculty of Engineering, University of Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal.
LEPABE - Laboratory for Process Engineering, Environment, Biotechnology and Energy, Faculty of Engineering, University of Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal.
Sci Total Environ. 2019 Feb 15;651(Pt 2):2606-2614. doi: 10.1016/j.scitotenv.2018.10.143. Epub 2018 Oct 11.
A Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) methodology followed by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) analysis was developed to extract synthetic musk compounds (SMCs) (6 polycyclic, 2 macrocyclic and 5 nitro musks) and ultraviolet-filters (UVFs) (6 compounds) from sludge. This methodology fills a gap in the literature, since the proposed technique does not require specific equipment, nor large amounts of solvents, sorbents and time to extract SMCs and UVFs from sludge. To optimize this new methodology, a design of experiments (DoE) approach was used, applying first a screening design (SD) and then a central composite design (CCD). The best conditions achieved to extract these 19 compounds simultaneously were: 500 mg freeze dried sludge, 2.5 min of vortex and 15 min ultrasound and the use of a QuEChERS for the dispersive solid-phase extraction (d-SPE) containing 500 mg MgSO, 410 mg C18 and 315 mg PSA. Then, this methodology was successfully validated. Recoveries of the target compounds ranged from 75% (cashmeran, DPMI) to 122% (2‑ethylhexyl 4‑methoxycinnamate, EHMC), with good repeatability (relative standard deviation < 10%). The instrumental detection limits (IDLs) and quantification (IQLs) varied from 0.001 pg (musk moskene, MM) to 7.5 pg (musk xylene, MX) and from 0.003 (MM) to 25 pg (MX), respectively. The method detection and quantification limits (MDLs and MQLs) ranged between 0.5 (DPMI) and 1394 (exaltolide, EXA) ng/g dw and 2 and 4648 ng/g-dw, respectively. Both SMCs and UVFs were detected in all sludge samples analysed. Higher concentrations were found for octocrylene (OC: maximum value of 115,486 ng/g-dw) followed by galaxolide (HHCB: 81,771 ng/g-dw). Only the nitro musks ambrette, xylene, moskene and tibetene and macrocyclic musk ethylene brassylate (EB) were not detected in any sample.
建立了一种快速、简便、廉价、有效、耐用和安全（QuEChERS）的方法，随后采用气相色谱-三重四极杆质谱法（GC-MS/MS）对污泥中的合成麝香化合物（SMCs）（6 种多环麝香、2 种大环麝香和 5 种硝基麝香）和紫外线滤光剂（UVFs）（6 种化合物）进行提取。该方法填补了文献中的空白，因为所提出的技术不需要特定的设备，也不需要大量的溶剂、吸附剂和时间来从污泥中提取 SMCs 和 UVFs。为了优化这种新方法，采用实验设计（DoE）方法，首先采用筛选设计（SD），然后采用中心组合设计（CCD）。为了同时提取这 19 种化合物，最佳条件为：500mg 冷冻干燥污泥、2.5min 涡旋和 15min 超声以及使用 QuEChERS 进行分散固相萃取（d-SPE），其中包含 500mg MgSO4、410mg C18 和 315mg PSA。然后，对该方法进行了成功验证。目标化合物的回收率为 75%（卡什米尔麝香、DPMI）至 122%（2-乙基己基 4-甲氧基肉桂酸酯、EHMC），重复性良好（相对标准偏差<10%）。仪器检测限（IDL）和定量限（IQL）分别为 0.001pg（麝香莫斯卡林、MM）至 7.5pg（麝香二甲苯、MX）和 0.003（MM）至 25pg（MX）。方法检测限（MDL）和定量限（MQL）分别为 0.5（DPMI）至 1394（倍半萜内酯、EXA）ng/gdw 和 2 至 4648ng/gdw。所有分析的污泥样品中均检测到 SMCs 和 UVFs。发现其中含量较高的是奥克立林（OC：最高值为 115486ng/gdw），其次是六氢-对二甲苯麝香（HHCB：81771ng/gdw）。只有硝基麝香、二甲苯麝香、莫斯卡林麝香和西藏麝香以及大环麝香乙基己基溴酸盐（EB）未在任何样品中检出。
