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藻源致嗅物质引起的水体嗅味是高藻源水环境的重要问题,其定量检测难度高,特别是胞内致嗅物质的检测容易出现误差。建立了顶空固相微萃取与气相色谱质谱联用技术(HS/SPME/GC/MS)同时定量检测水中5种典型藻源致嗅物质β-环柠檬醛、β-紫罗兰酮、二甲基三硫醚、2-甲基异莰醇和土臭素的方法,各物质标准曲线的线性关系良好(R2>0.99),检测限显著低于其嗅阈值,回收率为92.60%~113.70%,相对标准偏差(RSD)≤5.92%。以铜绿微囊藻为例,建立了用于胞内致嗅物质检测的加热盐浴前处理方法。采用密封萃取瓶内加热盐浴处理藻液,检测藻液中致嗅物质总含量,以总含量与经0.45μm滤膜过滤后胞外含量的差值作为胞内含量。流式细胞技术检测表明,HS/SPME预热3 min内,破胞率超过99%。激光粒度仪检测发现藻细胞以穿孔方式破胞同时细胞尺寸未发生明显变化。加热盐浴差值法简化了操作,缩短了破胞处理时间,密封环境下破胞降低挥发损失,从而保证了胞内致嗅物质检测的准确性。
Algae caused by olfactory substances caused by the smell of water is an important issue in the high algal source water environment, the quantitative detection of high difficulty, especially intracellular detection of olfactory substances prone to error. The headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry (HS / SPME / GC / MS) was developed for simultaneous determination of β-ring citral, β-ionone, Trichloride, trisulfide, 2-methylisothiol and geosmin. The calibration curve of each substance has good linearity (R2> 0.99), and the detection limit is significantly lower than its olfactory threshold (92.60% -113.70%). The relative standard Deviation (RSD) ≤ 5.92%. Taking Microcystis aeruginosa as an example, a heated salt bath pretreatment method for the detection of intracellular olfactory substances was established. The algae liquid was treated with the heated salt bath in a sealed extraction bottle to measure the total content of olfactory substances in the algae liquid. The difference between the total content and the extracellular content after filtration through 0.45 μm membrane was taken as the intracellular content. Flow cytometry showed HS / SPME preheated within 3 min, the breaking rate of more than 99%. The laser particle size analyzer detected that the algae cells were perforation-disrupted while the cell size did not change significantly. Difference heating salt bath method simplifies the operation, reducing the processing time, breaking the seal under the environment to reduce evaporation loss, thus ensuring the detection of intracellular olfactory substance accuracy.