固相萃取气相色谱-质谱联用法同时测定水中116种半挥发性有机物.docVIP

固相萃取/气相色谱-质谱联用法同时测定水中116种半挥发性有机物 郑能雄 林华影 柯 华 徐幽琼 盛丽娜 李一丹 张 琼 林 瑶 王春兰 林 侃 肖明发 （福建省福州市疾病预防控制中心，福建福州 350004） [摘 要] 目的：建立固相萃取/气相色谱-质谱联用同时测定水中116种半挥发性有机物的方法。方法：采用C18固相萃取柱富集吸附水样中的目标组分，以二氯甲烷和乙酸乙酯洗脱浓缩，DB-5MS毛细管柱分离，采用气相色谱-质谱联用的全扫描模式进行分析，选择特征离子定量。结果：能简便、快速、有效地分离检测水中的116种半挥发性有机物，方法的线性范围宽，相关系数大于0.9961，响应因子的相对标准偏差小于4.92％，样品加标回收率在81.6％～119.8％之间。结论：本法具有较高的选择性、灵敏度和准确度，对多种水样适应性好，适合水中116种半挥发性有机物的同时检测分析。 [关键词] 固相萃取；气相色谱-质谱法；水；半挥发性有机物 [中图分类号] O657.63 O659.37 [文献标识码] A Simultaneous determination of 116 kinds of semi-volatile organic compounds in water by gas chromatography／mass spectrometry with solid phase extraction Zheng Nen-gxiong, Lin Hua-ying, Ke Hua, Xu You-qiong, Sheng-Li-na，Li Yi-dan, Zhang Qiong, Lin Yao, Wang Chun-lan, Lin Kan, Xiao Ming-fa （Fuzhou disease prevention and control center, Fu Zhou, 350004, China） [Abstract] Objective: To establish a method for simultaneous determination of 116 kinds of semi-volatile organic compounds in water by gas chromatography／mass spectrometry with solid-phase extraction. Methods: Water sample was extracted on Cl8 solid phase column and eluted with dichloromethane ethyl acetate then separated by GC with an DB-5 MS capillary column. The interest analyses were analyzed by gas chromatography／mass spectrometry used all scan mode. Selective ion masses were used in quantitative measurement. Results: Enable to easily and effectively separate and determinate 116 kinds of semi-volatile organic compounds in water. In this method, broad linearity range, good linearity which correlation coefficient was greater than 0.9961, RF RSD was less than 4.92％,the average recoveries rates were between 81.6% and 119.8%. Conclusions: This method established was so selective and sensitive and exact. It has good adaptility to various water samples. It is suitable for simultaneous determination of 116 kinds of semi-volatile organic compounds in water. [Key words] solid phase extraction; gas chromatography/mass spectrometry ; water ; semi-volatile or