Department of Chemistry, National Central University, Chung-Li, Taiwan.
J Sep Sci. 2012 Aug;35(16):2122-30. doi: 10.1002/jssc.201200146.
A rapid and solvent-free procedure for the determination of 4-tert-octylphenol and 4-nonylphenol isomers in aqueous samples is described. The method involves in-situ acetylation and microwave-assisted headspace solid-phase microextraction prior to their determination using gas chromatography-ion trap mass spectrometry operated in the selected ion storage mode. The dual experimental protocols to evaluate the effects of various derivatization and extraction parameters were investigated and the conditions optimized. Under optimized conditions, 300 μL of acetic anhydride mixed with 1 g of potassium hydrogencarbonate and 2 g of sodium chloride in a 20 mL aqueous sample were efficiently extracted by a 65 μm polydimethylsiloxane-divinylbenzene fiber that was located in the headspace when the system was microwave irradiated at 80 W for 5 min. The limits of quantitation were 5 and 50 ng/L for 4-tert-octylphenol and 4-nonylphenol isomers, respectively. The precision for these analytes, as indicated by relative standard deviations, were less than 8% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was between 74 to 88%. A standard addition method was used to quantitate 4-tert-octylphenol and 4-nonylphenol isomers, and the concentrations ranged from 120 to 930 ng/L in various environmental water samples.
描述了一种快速、无溶剂的方法，用于测定水样中 4-叔辛基苯酚和 4-壬基酚异构体。该方法涉及原位乙酰化和微波辅助顶空固相微萃取，然后使用气相色谱-离子阱质谱在选择离子存储模式下进行测定。研究了两种实验方案以评估各种衍生化和提取参数的影响，并对条件进行了优化。在优化条件下，将 300 μL 乙酸酐与 1 g 碳酸氢钾和 2 g 氯化钠混合，在 20 mL 水样中，当系统在 80 W 下微波辐射 5 min 时，将其置于顶空的 65 μm 聚二甲基硅氧烷-二乙烯基苯纤维中进行有效萃取。4-叔辛基苯酚和 4-壬基酚异构体的定量限分别为 5 和 50 ng/L。这些分析物的精密度（以相对标准偏差表示），无论是日内还是日间分析，均小于 8%。准确度以平均萃取回收率表示，在 74%至 88%之间。采用标准加入法对各种环境水样中的 4-叔辛基苯酚和 4-壬基酚异构体进行定量，浓度范围为 120 至 930 ng/L。
