气相色谱-质谱联用同时测定沉积物中三氯生和甲基三氯生

Simultaneous determination of triclosan and methyl-triclosan in sediments by gas chromatography coupled with mass spectrometry

建立了气相色谱-质谱联用（GC-MS）技术同时分析沉积物中三氯生和甲基三氯生的方法。采用丙酮提取沉积物样品,提取物经自制C18固相萃取柱净化,利用N-甲基-N（三甲基硅）-三氟乙酰胺（MSTFA）对提取物中三氯生进行衍生化,用外标法进行定量。GC-MS对三氯生和甲基三氯生的检出限分别为0.59ng/g和0.28ng/g,沉积物中三氯生和甲基三氯生不同浓度的加标回收率分别为85.6%-95.7%和84.4%-106.7%,相对标准偏差（RSD）分别为3.5%-6.9%和3.9%-6.3%。对6个沉积物样品进行了分析测定,三氯生和甲基三氯生的浓度分别为12.41-93.77ng/g和4.96-6.48ng/g。研究结果表明,该方法适用于同时测定沉积物样品中三氯生和甲基三氯生的含量,具有检出限低、灵敏度高、重复性好等优点,是一个较为可靠的检测方法。

A method is developed for simultaneous analysis of triclosan（TCS）and methyl-triclosan（MTCS）by using gas chromatography coupled with mass spectrometry（GC-MS）.Samples are extracted with actone,and then cleaned-up with a C18solid-phase extraction cartridge.TCS in the extracts is derivatized with N-methylN（trimethylsilyl）-trifluoroacetamide（MSTFA）,and then quantitatively analyzed by using the external standard method.The limits of detection（LOD）are 0.59 ng/g and 0.28 ng/g for TCS and MTCS,respectively.The spiked recoveries of TCS and MTCS are 85.6%- 95.7% and 84.4%- 106.7%,respectively.And the relative standard deviation（RSD）is in the range of 3.5%-6.9% and 3.9%-6.3%for TCS and MTCS,respectively.TCS and MTCS are determined by the optimized method in six sediment samples,and the concentrations are 12.41-93.77 ng/g and 4.96-6.48 ng/g for TCS and MTCS,respectively.The results indicate that the method is a reliable detection method with low detection limit,high sensitivity and repeatability for simultaneous determination of TCS and MTCS in sediments.