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使用Agilent1260型高效液相色谱仪,建立定量测定天然水体中5种微囊藻毒素(MC-RR、YR、LR、LA、LY)的分析方法。比较甲醇/三氟乙酸(TFA)水溶液与甲醇/磷酸两种流动相体系,待测物质的响应程度,结果发现,TFA作为缓冲溶液时,基线较磷酸稳定,因此,选择甲醇/TFA水溶液作为流动相。比较不同TFA体积比例,待测物质的分离程度,结果显示,甲醇/0.02%的TFA水溶液作为流动相时,5种MCs含量的分离度较好。比较等度和梯度洗脱条件,发现,梯度洗脱条件5种MCs的分离度较等度洗脱条件好。该方法 MC-RR、YR、LR、LA、LY的最低检出限(LOD)分别为0.015、0.035、0.018、0.032和0.026μg/L,最低定量限(LOQ)分别是0.049、0.117、0.062、0.106和0.086μg/L。在0.10～1.50μg/mL的线性范围内,相关系数R2≥0.99,实际水样回收率为73.9%～103.3%。
An analytical method for the quantitative determination of 5 microcystin (MC-RR, YR, LR, LA, LY) in natural waters was established using an Agilent 1260 HPLC. A comparison of methanol / trifluoroacetic acid (TFA) aqueous solution with methanol / phosphoric acid mobile phase system and the degree of response of the substance to be tested revealed that when TFA was used as a buffer solution, the base line was more stable than phosphoric acid. Therefore, methanol / TFA aqueous solution was selected as a mobile phase. The volume fraction of different TFA and the degree of separation of the tested substances were compared. The results showed that the separation of five kinds of MCs was better when using methanol / 0.02% TFA as mobile phase. Compared with isocratic and gradient elution conditions, it was found that the separation conditions of five kinds of MCs under gradient elution conditions are better than that of isocratic elution. The minimum detectable limit (LOD) of MC-RR, YR, LR, LA and LY were 0.015,0.035,0.018,0.032 and 0.026μg / L respectively. The LOQs were 0.049,0.117,0.062, 0.106 and 0.086 μg / L. In the linear range of 0.10 ~ 1.50μg / mL, the correlation coefficient R2≥0.99, the actual water sample recovery was 73.9% ~ 103.3%.