藻毒素MC-RR的高效液相色谱检测方法摸索及上海水体中MC-RR的定性研究

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摘要：本实验拟通过摸索利用HPLC建立藻毒素MC-RR的检测方法，在色谱柱为：Boston Green ODS 250 mm×4.6 mm，5 μm C18柱，流速为：1mL/min，柱温为：25°C，进样量为：10μL，检测波长为：238nm的条件下尝试不同的流动相配比（甲醇：水=60:40和乙腈：水=75:25）对MC-RR标准样品进行分析，发现乙腈要比甲醇对于洗脱MC-RR灵敏度要高。并同期对MC-LR标准样品进行检测对比，实验发现，相同流动相下（乙腈：水=75:25）对洗脱MCs的灵敏度有一定差别，对MC-RR灵敏度一般，线性范围0.94-0.96，对MC-LR灵敏度较高，线性符合要求。通过高效液相色谱法对MC-RR的检测方法摸索发现，本实验条件下HPLC法对MC-RR的检测灵敏度未达到高效液相的检测标准，但能通过标线初步估计浓度，具有一定的参考价值，得到一些初步的结论，需进一步探索更完善的实验方法。对2017年3月的上海市天潼路苏州河等五个地区的典型水体进行采样及预处理，并对水样当中的MC-RR进行定性研究，并初步定量分析。实验发现，天潼路苏州河、徐汇区莲花路和闵行区剑川路实际水体中存在MC-RR，MCs浓度分别为0.17μg/L、0.33μg/L、2.26μg/L，其中闵行区剑川路已经高于地表水中MCs含量的最低限度1μg/L，证明郊区水体较于市区水体要污染严重。常规水处理工艺不能有效地去除水中的微囊藻毒素，需要加强对水体水质的检测，因而分析研究MC-RR的准确测定方法有重要意义。70035

关键词：铜绿微囊藻；微囊藻毒素；高效液相色谱法；固相萃取

Study on the Detection of Microcystin MC-RR by High Performance Liquid Chromatography and qualitative study on MC - RR in Shanghai Water

Abstract: In this experiment, the detection method of algal toxin MC-RR was established by HPLC. The column was: Boston Green ODS 250 mm × 4.6 mm, 5 μm C18 column, flow rate: 1 mL / min, column temperature: 25 ° C (Methanol: water = 60: 40 and acetonitrile: water = 75: 25) were used to analyze the MC-RR standard sample, and the acetonitrile It is higher than methanol for elution MC-RR. (Acetonitrile: water = 75: 25) had a certain sensitivity to eluted MCs. The sensitivity of MC-RR was linear, and the linear range was 0.94-0.96. The sensitivity of MC-LR was similar to that of MC-LR standard sensitivity is higher, linear meet the requirements. The detection sensitivity of MC-RR by HPLC was not up to the standard of high performance liquid chromatography, but it could be used to estimate the concentration of MC-RR by high performance liquid chromatography. Reference value, get some preliminary conclusions, need to further explore a more complete experimental method. The typical water bodies in five areas of Tiantong Road, Shanghai, and so on in March 2017 were sampled and pretreated, and the MC-RRs in water samples were qualitatively studied and quantitatively analyzed. The results showed that MC-RR and MCs concentrations were 0.17μg/L, 0.33μg/L and 2.26μg/L, respectively, and the concentration of MC-RR and MCs in Liuhua River, Xuhua District, Xuhui District and Minhang District, Has been higher than the surface water MCs content of the minimum 1μg/L, proved suburban water than urban water pollution. Conventional water treatment process can not effectively remove microcystins in water, and it is necessary to strengthen the detection of water quality. Therefore, it is important to analyze the method of accurate determination of MC-RR.

Keywords: Microcystis aeruginosa; Microcystin; HPLC; SPE

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