Citation: ZHOU Li, DONG Liang, SHI Shuangxin, ZHANG Lifei, ZHANG Xiulan, YANG Wenlong, LI Lingling, HUANG Yeru. Determination of kepone in water by liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(3): 211-215. doi: 10.3724/SP.J.1123.2013.11053 shu

Determination of kepone in water by liquid chromatography-tandem mass spectrometry

1.
National Research Center for Environmental Analysis & Measurement, Beijing 100029, China

Corresponding author: HUANG Yeru,
Received Date: 28 November 2013
Available Online: 13 January 2014
Fund Project: 2010年环境保护重大公益专项(20100902601) (20100902601)2010年科技部创新方法研究专项(2010IM031000). (2010IM031000)

An analytical procedure for the determination of kepone in water was described. Water samples were extracted by liquid-liquid extraction, and then cleaned-up. Chromatographic separation was performed on an Eclipse plus C18 column (100 mm×2.1 mm, 3.5 μm) with gradient elution using acetonitrile and water at a flow rate of 0.3 mL/min. The target compounds were determined in multiple reaction monitoring (MRM) mode via negative electrospray ionization (ESI^-) and quantified by isotopic-dilution technique. Results showed that kepone existed as diol form and hemiacetal in acetone/acetonitrile and methanol respectively, the structures of which were confirmed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Due to the polar nature of kepone, it was difficult to be eluted during clean-up procedure and it may be decomposed during sulfuric acid washing. Therefore, it could not be analyzed together with the other organochlorine pesticides. The calibration curve showed good linearity in the range of 5-100 μg/L with correlation coefficient (r²) of 0.999. The limit of detection was 0.70 ng/L and the limit of quantification was 2.8 ng/L in water. The average recoveries when spiked at 5, 40 and 100 ng/L in water were 95.1%-98.9%, and the relative standard deviations (RSDs) were 3.85%-4.72%. The method can be used to the determination of kepone in water due to its high sensitivity, good recovery and reproducibility.
- high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS),
- kepone,
- water
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