Citation: YU Rui-Peng, WANG Li-Ping, ZHAO Chen-Kai, WU Sheng-Fang, SONG Qi-Jun. Determination of Volatile Metabolites in Microcystis Aeruginosa Using Headspace-Solid Phase Microextraction Arrow Combined with Gas Chromatography-Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2020, 48(6): 750-756. doi: 10.19756/j.issn.0253-3820.191616 shu

Determination of Volatile Metabolites in Microcystis Aeruginosa Using Headspace-Solid Phase Microextraction Arrow Combined with Gas Chromatography-Mass Spectrometry

1.
School of Chemical and Material Engineering, Jiangnan University, Wuxi 214122, China;
2.
State Key Laboratory of Food Science and Technology, Jiangnan University, Wuxi 214122, China

Received Date: 19 October 2019
Revised Date: 20 January 2020

Fund Project: This work was supported by the National Natural Science Foundation of China (No.51973083).

A novel headspace solid phase microextraction arrow (HS-SPME Arrow) method combined with gas chromatography-mass spectrometry (GC-MS) was developed for extraction and analysis of volatile organic compounds of Microcystis aeruginosa under simulated natural conditions. By selecting suitable extraction fibers, 210 kinds of volatile metabolites were identified by full scanning qualitative analysis from the samples of Microcystis aeruginosa in producing period. The metabolic changes of volatile molecules during the growth of Microcystis aeruginosa were analyzed by multivariate statistical analysis and clustering analysis. Chemometric analysis based on principal component analysis, partial least squares-discriminant analysis and heatmap associated with hierarchical cluster analysis provided a suitable tool to differentiate volatile organic compounds in algal material. And 10 metabolites in statistical significance were identified, including cyclohexanol, dimethyl trisulfide, benzenemethanol, camphor, 2-methoxyphenol, 3-hexene-1-ol, 2,4-decadienal, indole, citral and 1-nonanol. Parameters affecting the extraction, such as extraction temperature, time and salt were carefully optimized. In addition, the analysis conditions, including desorption temperature and time as well as gas chromatographic parameters, were optimized. The calibration curves showed a good linearity (correlation coefficient > 0.998) in the concentration range of 0.050-1000 ng/L. The detection limits of this method were 0.010-0.030 ng/L, and the recoveries at the concentration level of 100 ng/L were 76.3%-3.0%. The method was satisfactorily precise, with the RSDs of less than 12.7%. The new method was simple, quick, stable, and applicable to complex matrices. It was suitable to the determination of volatile metabolites in natural water at the early stage of blue-green algae bloom.
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沈阳化工大学材料科学与工程学院沈阳 110142