Necibi Mouna, Lanceleur Laurent, Mzoughi Nadia, Monperrus Mathilde
Faculté des Sciences de Tunis, Department de Chimie, Université de Tunis EL Manar, 1007, Tunis, Tunisia.
Laboratoire Milieu Marin, Institut National des Sciences et Technologies de la Mer, port de pêche, 2060, La Goulette, Tunisia.
Bull Environ Contam Toxicol. 2016 Nov;97(5):659-669. doi: 10.1007/s00128-016-1935-z. Epub 2016 Oct 14.
A new analytical method for the simultaneous determination of eight synthetic musks compounds (SMs) including five polycyclic musks (PCMs) and three nitro musks (NMs) was validated for sediment samples based on a simple QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation procedure followed by gas chromatography-mass spectrometry (GC-MS). Good analytical performances were obtained for all the target compounds. For the validation of the method, internal calibration (IC) and internal calibration with QuEChERS (ICQ) were compared. Good linearity was obtained for both calibration methods with determination coefficients (R) ranging between 0.990 for Musk Xylene (MX) and 0.999 for Tonalide (AHTN) with IC and between 0.991 for Musk Ketone (MK) and 0.999 for Traseolide (ATII) with ICQ. The repeatability ranges were 0.1 %-1.9 % with the IC and 0.1 %-2.6 % with the ICQ. The apparent recoveries obtained for SMs in the standard reference sediment (SRM1944) varied in the range of 70 %-98 % and 75 %-103 % in the sediment from the Bizerte Lagoon (Tunisia). The absolute recoveries ranged between 61 % and 92 % for the SRM1944 and between 61 % and 89 % in the sediment from the Bizerte Lagoon. The limits of detection (LOD) calculated for the two main compounds, Galaxolide (HHCB) and Tonalide (AHTN) were 0.3 and 0.1 ng g respectively. The LODs obtained for ADBI (Celestolide), AHMI (Phantolide), ATII (Traseolide), MM (Muks mosken), MK (Musk Ketone) and MX (Musk Xylene) were 0.08, 0.12, 0.03, 0.34, 0.11, 0.08, 0.10 and 0.15 ng g respectively. The levels of ∑SMs in surface sediments from the Bizerte Lagoon ranged from 1.4 to 4.5 ng g, which are 1000 times lower that the predicted no effect concentration (PNEC) for marine organisms.
基于简单的QuEChERS(快速、简便、廉价、有效、耐用且安全)样品制备程序结合气相色谱-质谱联用(GC-MS)技术,建立了一种同时测定8种合成麝香化合物(SMs)的新分析方法,其中包括5种多环麝香(PCMs)和3种硝基麝香(NMs),并对沉积物样品进行了方法验证。所有目标化合物均获得了良好的分析性能。在方法验证过程中,比较了内标法(IC)和基于QuEChERS的内标法(ICQ)。两种校准方法均具有良好的线性,内标法中二甲苯麝香(MX)的决定系数(R)为0.990,吐纳麝香(AHTN)为0.999;基于QuEChERS的内标法中酮麝香(MK)的决定系数为0.991,佳乐麝香(ATII)为0.999。内标法的重复性范围为0.1% - 1.9%,基于QuEChERS的内标法为0.1% - 2.6%。在标准参考沉积物(SRM1944)中获得的SMs表观回收率在70% - 98%之间,在突尼斯比塞大泻湖沉积物中为75% - 103%。SRM1944的绝对回收率在61% - 92%之间,比塞大泻湖沉积物中为61% - 89%。两种主要化合物, galaxolide(HHCB)和吐纳麝香(AHTN)的计算检出限(LOD)分别为0.3和0.1 ng/g。ADBI(celestolide)、AHMI(phantolide)、ATII(traseolide)、MM(muks mosken)、MK(酮麝香)和MX(二甲苯麝香)的检出限分别为0.08、0.12、0.03、0.34、0.11、0.08、0.10和0.15 ng/g。比塞大泻湖表层沉积物中∑SMs的含量范围为1.4至4.5 ng/g,比海洋生物的预测无效应浓度(PNEC)低100倍。