PDF《固相微萃取/ 高效液相色谱联用分析 水样中邻苯二甲酸酯》

第24卷第5期 分析测试学报 Vol.

24 No.

5 2005年 9月 FENXI CESHI XUEBAO( Journal of Instrumental Analysis) 35~

38 研究简报 固相微萃取/ 高效液相色谱联用分析 水样中邻苯二甲酸酯 王超英, 李碧芳, 李攻科 ( 中山大学 化学与化学工程学院, 广东 广州 510275) 摘要: 研究了固相微萃取( SPME) / 高效液相色谱( HPLC) 联用测定环境中痕量邻苯二甲酸酯的分析方法. 比较 了5种不同类型涂层对

5 种邻苯二甲酸酯的萃取效果, 采用

3 因素

3 水平正交实验设计对 SPME 的条件如萃取时 间, 离子强度, 解吸时间等进行了优化. SPME 优化的条件为:

65 Lm 聚二甲基硅烷/ 乙烯苯( PDMS/ DVB) 涂层, 室温, 搅拌速率

1 100 r/ min, 萃取时间

30 min, 纯乙腈解吸, 解吸时间

2 min. HPLC 的条件: C18 反相色谱柱, 乙腈- 水( 体积比

60 B40) 梯度淋洗, 流速

1 mL/ min, 紫外检测波长

228 nm. 方法的线性范围为 0. 50~ 80.

00 Lg/ L, 检出限为 0. 11~ 2.

20 Lg/ L, 相对标准偏差( n= 6) 为2. 5% ~ 9. 6% . 用于自来水、 凉开水和雨水等实际水样的分 析, 回收率为 82% ~ 128% . 关键词: 固相微萃取;

高效液相色谱;

邻苯二甲酸酯;

水样 中图分类号: O657;

O658 文献标识码: A 文章编号: 1004- 4957( 2005) 05- 0035-

04 Determination of Phthalate Esters in Water Samples by Solid_phase Microextraction and High Performance Liquid Chromatography WANG Chao_ying, LI Bi_fang, LI Gong_ke ( Chemistry and Chemical Engineering School, Sun Yat_sen University, Guangzhou 510275, China) Abstract: A solid_phase microextraction( SPME) method coupled with HPLC/ UV was developed and validated for the determination of five phthalate esters( dimethyl_, diethyl_, di_n_butyl_, butylbenzyl_, di_2_ethy- l hexyl_ and di_n_octyl phthalate) in water samples. Five different types of SPME polymer coatings were inves - tigated. On the basis of orthogonal experiments with three factors, three levels and nine groups, the SPME experimental conditions, such as extraction time, effects of ion strength, and thermal desorption time were optimized. The optimized parameters for the SPME method were as follows:

65 Lm PDMS/ DVB fiber, room temperature, stirring rate of

1 100 r/ min, extraction time of

30 min, thermal desorption time of

5 min, and use of acetonitrile as desorption solution. Acetonitrile- water(

60 B

40 by volume) was used as the mobile phase with gradient elution on the C18 reversed phase chromatography column, and the flow rate was

1 mL/ min. The detection wavelength was

228 nm with the UV- VIS detector. The linear range of the method was determined to be from0.

50 to 80.

00 Lg/ L, and the detection limit varied from 0.

11 to 2.

20 Lg/ L. The rela - tive standard deviation( n= 6) was 2. 5% - 9. 6% . This method was used for determination of phthalate es - ters in water sample, such as tap, boiled and rain water, and the recoveries ranged from 82% to 128% . The method is fast, convenient, sensitive, solvent_free, and suitable for the determination of trace phthalate esters in environmental water samples. Key words: Solid_phase microextraction;

High_performance liquid chromatography;

Phthalate esters;

Water sample 邻苯二甲酸酯是农药载体、驱虫剂、 化妆品、香味品、润滑剂和去泡剂的生产原料, 在家具、 汽车、 电线电缆、服装等行业也有广泛的应用. 由于邻苯二甲酸酯的大量使用对生态环境造成了污染. 邻苯 收稿日期: 2004- 08- 09;