State Key Laboratory of Organic Geochemistry, CAS Centre for Pearl River Delta Environmental Pollution and Control Research, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, China.
Anal Bioanal Chem. 2012 Dec;404(10):3175-88. doi: 10.1007/s00216-012-6444-2. Epub 2012 Oct 10.
A sensitive and robust method using solid-phase extraction and ultrasonic extraction for preconcentration followed by ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS-MS) has been developed for determination of 19 biocides: eight azole fungicides (climbazole, clotrimazole, ketoconazole, miconazole, fluconazole, itraconazole, thiabendazole, and carbendazim), two insect repellents (N,N-diethyl-3-methylbenzamide (DEET), and icaridin (also known as picaridin)), three isothiazolinone antifouling agents (1,2-benzisothiazolinone (BIT), 2-n-octyl-4-isothiazolinone (OIT), and 4,5-dichloro-2-n-octyl-isothiazolinone (DCOIT)), four paraben preservatives (methylparaben, ethylparaben, propylparaben, and butylparaben), and two disinfectants (triclosan and triclocarban) in surface water, wastewater, sediment, sludge, and soil. Recovery of the target compounds from surface water, influent, effluent, sediment, sludge, and soil was mostly in the range 70-120%, with corresponding method quantification limits ranging from 0.01 to 0.31 ng L(-1), 0.07 to 7.48 ng L(-1), 0.01 to 3.90 ng L(-1), 0.01 to 0.45 ng g(-1), 0.01 to 6.37 ng g(-1), and 0.01 to 0.73 ng g(-1), respectively. Carbendazim, climbazole, clotrimazole, methylparaben, miconazole, triclocarban, and triclosan were detected at low ng L(-1) (or ng g(-1)) levels in surface water, sediment, and sludge-amended soil. Fifteen target compounds were found in influent samples, at concentrations ranging between 0.4 (thiabendazole) and 372 ng L(-1) (methylparaben). Fifteen target compounds were found in effluent samples, at concentrations ranging between 0.4 (thiabendazole) and 114 ng L(-1) (carbendazim). Ten target compounds were found in dewatered sludge samples, at concentrations ranging between 1.1 (DEET) and 887 ng g(-1) (triclocarban).
已开发出一种使用固相萃取和超声萃取进行预浓缩的灵敏且稳健的方法，然后采用超高效液相色谱-串联质谱法（UHPLC-MS-MS）对 19 种杀生物剂进行测定：八种唑类杀菌剂（克霉唑、氯己定、酮康唑、咪康唑、氟康唑、伊曲康唑、噻苯达唑和多菌灵）、两种驱虫剂（N,N-二乙基-3-甲基苯甲酰胺（DEET）和羟哌啶（也称为派卡瑞丁））、三种异噻唑啉酮防污剂（1,2-苯并异噻唑啉-3-酮（BIT）、2-正辛基-4-异噻唑啉-3-酮（OIT）和 4,5-二氯-2-正辛基异噻唑啉-3-酮（DCOIT））、四种对羟基苯甲酸酯防腐剂（对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯和对羟基苯甲酸丁酯）和两种消毒剂（三氯生和三氯卡班）在地表水、废水、沉积物、污泥和土壤中。从地表水、进水、出水、沉积物、污泥和土壤中回收目标化合物的回收率大多在 70-120%之间，相应的方法定量限范围为 0.01-0.31ng/L、0.07-7.48ng/L、0.01-3.90ng/L、0.01-0.45ng/g、0.01-6.37ng/g 和 0.01-0.73ng/g。在地表水、沉积物和添加污泥的土壤中，以低 ng/L（或 ng/g）水平检测到多菌灵、克霉唑、克霉唑、对羟基苯甲酸甲酯、咪康唑、三氯卡班和三氯生。在进水样品中发现了 15 种目标化合物，浓度范围为 0.4（噻菌灵）至 372ng/L（对羟基苯甲酸甲酯）。在出水样品中发现了 15 种目标化合物，浓度范围为 0.4（噻菌灵）至 114ng/L（多菌灵）。在脱水污泥样品中发现了 10 种目标化合物，浓度范围为 1.1（DEET）至 887ng/g（三氯卡班）。
