Analytical Sciences

Development of Miniaturized Hollow-fiber Assisted Liquid-phase Microextraction with in situ Acyl Derivatization Followed by GC-MS for the Determination of Benzophenones in Human Urine Samples

Rie Ito,* Migaku Kawaguchi,** Youji Koganei,* Hidehiro Honda,* Noriya Okanouchi,* Norihiro Sakui,*** Koichi Saito,* and Hiroyuki Nakazawa*

*Department of Analytical Chemistry, Faculty of Pharmaceutical Sciences, Hoshi University, 2-4-41 Ebara, Shinagawa, Tokyo 142-8501, Japan
**Bio-Medical Standard Section, National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba Central 3, 1-1-1 Umezono, Tsukuba, Ibaraki 305-8563, Japan
***Agilent Technologies, Hachioji Site, 9-1 Takakura, Hachioji, Tokyo 192-0033, Japan

A simple and highly sensitive method that involves miniaturized hollow fiber assisted liquid-phase microextraction (HF-LPME) with in situ acyl derivatization and GC-MS was developed for the determination of benzophenone (BP) and related compounds in human urine samples. The limits of detection (S/N = 3) and quantification (S/N > 10) of BPs in human urine samples are 0.01 to 0.05 and 0.05 to 0.2 ng ml⁻¹, respectively. The average recoveries of BPs (n = 5) in human urine samples spiked with 10 and 50 ng ml⁻¹ BPs are 93.1 to 106.7% (RSD: 1.5 to 8.4%) and 96.3 to 101.5% (RSD: 3.0 to 7.7%), respectively. When the proposed method was applied to human urine samples, BPs were detected at the sub ng ml⁻¹ level.

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