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目的:建立蝉翼藤中4个酮类化合物的HPLC定量测定方法。方法:采用Symmetry-C_(18)(4.6 mm×250 mm,5μm)色谱柱,以甲醇(A)-0.1%甲酸水溶液(B)为流动相,梯度洗脱(0~25 min,50%A→55%A;25~35 min,55%A→65%A;35~40 min,65%A),流速1.0 m L·min~(-1),柱温30℃,检测波长265 nm。结果:7-羟基-1,2-二甲氧基(口山)酮、1,7-二羟基-4-甲氧基(口山)酮、2-羟基-1,7-二甲氧基(口山)酮、1,7-二羟基(口山)酮进样量分别在0.048 2~0.241、0.063~0.315、0.052 4~0.262和0.106 6~0.533μg范围内与峰面积呈良好线性关系(r>0.999 0);平均加样回收率分别为100.4%、98.9%、100.2%、101.1%,RSD为别为1.8%、1.7%、1.8%、2.0%。不同来源的3个样品中7-羟基-1,2-二甲氧基(口山)酮、1,7-二羟基-4-甲氧基(口山)酮、2-羟基-1,7-二甲氧基(口山)酮、1,7-二羟基(口山)酮的含量范围分别为47.37~54.73、65.72~99.69、64.05~87.26、163.2~195.6μg·g~(-1)。结论:经方法学验证,本法可用于蝉翼藤中4个酮的含量测定。
Objective: To establish a method for the quantitative determination of 4 chironones in Cicada vinescens by HPLC. METHODS: Symmetry-C_ (18) (4.6 mm × 250 mm, 5 μm) column was used with a mobile phase of methanol (A) -0.1% formic acid (B) → 55% A; 25-35 min; 55% A → 65% A; 35-40 min, 65% A) at a flow rate of 1.0 m L · min -1. Results: 7-Hydroxy-1,2-dimethoxycholanone, 1,7-dihydroxy-4-methoxycholanone, 2-hydroxy-1,7-dimethoxy (Kusan) Ketone and 1,7-dihydroxy (Kusama) Ketone showed a good linear relationship with the peak area in the range of 0.048 2-0.241, 0.063-0.315, 0.052 4-0.262 and 0.106 6-0.533 μg, respectively (r> 0.999 0). The average recoveries were 100.4%, 98.9%, 100.2% and 101.1% respectively. The RSDs were 1.8%, 1.7%, 1.8% and 2.0% respectively. Among the three samples from different sources, 7-hydroxy-1,2-dimethoxycholanone, 1,7-dihydroxy-4-methoxycholanone, 2-hydroxy- (Kusan) ketone, 1,7-dihydroxy (Kusan) ketone in the range of 47.37 ~ 54.73, 65.72 ~ 99.69, 64.05 ~ 87.26 and 163.2 ~ 195.6μg · g ~ . Conclusion: This method can be used to determine the content of 4 ketones in Cicadaera virens by methodological verification.