Determination of Microcystins in Aqueous Samples by Modified Solid-Supported Liquid Extraction combined with Liquid Chromatography-Tandem Mass Spectrometry

• Main Authors: Chang-Lin Hsu, 許暢麟
• Other Authors: Maw-Rong Lee
• Format: Others
• Language: zh-TW
• Published: 2015
• Online Access: http://ndltd.ncl.edu.tw/handle/34548787616207793423

碩士 === 國立中興大學 === 化學系所 === 103 === In this study, a rapid, simple, and sensitive analytical method was developed for the determination of the trace microcystins in water samples using solid-supported liquid extraction combined with liquid chromatography-tandem mass spectrometry (SLE-LC-MS/MS). Microcystin-LR (MC-LR), Microcystin-YR (MC-YR), and Microcystin-RR (MC-RR) are separated by C18 column and quantified by selected reaction monitoring (SRM) mode. The optimized extraction conditions for extracting of microcystins from water sample were using 100 mg diatomaceous earth as adsorption sorbent, 15 mL of methanol containing 5% formic acid as desorption solvent. The linearity of the proposed method was 0.5-100 ng/mL with the coefficients of determination (R2) above 0.9933. Limit of quantification (LOQ) and limit of detection (LOD) of three microcystins were between 0.4-0.7 ng/mL and 0.1-0.2 ng/mL, respectively. The intra-day and inter-day precision were between 0.7-5.8% and 5.3-16.7%, respectively. The recovery of the proposed method for analyzing of microcystins in water samples was between 89.5-106.6%. The analyses of trace microcysins in real water samples were also determined, the MC-RR was detected in the aquarium water at the concentration of 3.3 ng/mL. The results demonstrate that the proposed method reduced the sample preparation time from 40 min to 10 min without sacrificing any sensitivity.