PMID- 24984458 OWN - NLM STAT- PubMed-not-MEDLINE DCOM- 20150901 LR - 20190923 IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 32 IP - 3 DP - 2014 Mar TI - [Determination of kepone in water by liquid chromatography-tandem mass spectrometry]. PG - 211-5 AB - 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 x 2.1 mm, 3.5 microm) 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 microg/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. FAU - Zhou, Li AU - Zhou L FAU - Dong, Liang AU - Dong L FAU - Shi, Shuangxin AU - Shi S FAU - Zhang, Lifei AU - Zhang L FAU - Zhang, Xiulan AU - Zhang X FAU - Yang, Wenlong AU - Yang W FAU - Li, Lingling AU - Li L FAU - Huang, Yeru AU - Huang Y LA - chi PT - English Abstract PT - Journal Article PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 EDAT- 2014/07/06 06:00 MHDA- 2014/07/06 06:01 CRDT- 2014/07/03 06:00 PHST- 2014/07/03 06:00 [entrez] PHST- 2014/07/06 06:00 [pubmed] PHST- 2014/07/06 06:01 [medline] AID - 10.3724/sp.j.1123.2013.11053 [doi] PST - ppublish SO - Se Pu. 2014 Mar;32(3):211-5. doi: 10.3724/sp.j.1123.2013.11053.