State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, 511 Kehua Street, Wushan, Tianhe District, Guangzhou, Guangdong, 510640, China.
Anal Bioanal Chem. 2016 Nov;408(28):8177-8193. doi: 10.1007/s00216-016-9924-y. Epub 2016 Sep 13.
A sensitive and selective quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction combined with dispersive solid-phase extraction (d-SPE) cleanup method was developed to simultaneously extract a wide range of personal care products (16 biocides, 4 synthetic musks, and 4 benzotriazoles) in fish muscle and liver tissues. In order to get satisfactory recoveries, different extraction parameters were optimized, including extraction salts and d-SPE materials, extraction solvents and acetic acid contents in organic phase, and the ratios of solvent and water. Ultra pressure liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry were used to analyze the target compounds in the extracts. Among the 24 personal care products, the recoveries in the range of 70-120 % were obtained for 20, 19, and 12 analytes in fish muscle at the spiking concentrations of 10, 5, and 1 ng/g ww, respectively, and for 13, 12, and 11 analytes in liver at the spiking concentrations of 40, 20, and 4 ng/g ww, respectively. Method quantification limits (MQLs) of all analytes were 0.02-2.12 ng/g ww for fish muscle and 0.22-12.2 ng/g ww for fish liver tissues. The method was successfully applied to wild fish samples collected from Dongjiang River, south China. Twenty-one and 17 of the analytes were found in fish muscle and liver samples, respectively, in at least one site of the river with the concentrations between below MQLs and 119 ng/g ww, respectively. Graphical abstract Achieved satisfactory recoveries, high precision, and low method quantification limits (MQLs) for PCPs in wild fish tissues by QuEChERS procedure optimization combined with UPLC-MS/MS and GC-MS analyses.
建立了一种灵敏、选择性强、快速、简便、价廉、有效、耐用且安全的(QuEChERS)提取方法,并结合分散固相萃取(d-SPE)净化方法,用于同时提取鱼类肌肉和肝脏组织中的多种个人护理产品(16 种杀菌剂、4 种合成麝香和 4 种苯并三唑)。为了获得满意的回收率,优化了不同的提取参数,包括提取盐和 d-SPE 材料、提取溶剂和有机相中乙酸的含量,以及溶剂和水的比例。采用超高效液相色谱-串联质谱法和气相色谱-质谱法分析提取物中的目标化合物。在所研究的 24 种个人护理产品中,在 10、5 和 1ng/g ww 的添加浓度下,20、19 和 12 种分析物在肌肉中的回收率范围为 70-120%,在 40、20 和 4ng/g ww 的添加浓度下,13、12 和 11 种分析物在肝脏中的回收率范围为 70-120%。所有分析物在肌肉中的方法定量限(MQLs)为 0.02-2.12ng/g ww,在肝脏中的 MQLs 为 0.22-12.2ng/g ww。该方法成功应用于中国南方东江采集的野生鱼类样本。在该河流的至少一个地点,在所采集的肌肉和肝脏样本中发现了 21 种和 17 种分析物,其浓度在 MQLs 与 119ng/g ww 之间。