目的 基于附子强心组分去甲乌药碱、去甲猪毛菜碱和棍掌碱共有的肾上腺素类似结构,构建了以邻二酚羟基基团与茜素红S-苯硼酸体系置换反应为核心的光化学比色传感器,用于整体评价附子配方颗粒的强心作用。方法 以传感器的响应强度为评价指标,对超声提取时间、料液比、提取液浓度和乙二胺四乙酸二钠(EDTA-2Na)浓度等供试品的制备条件进行优化;并对该方法的精密度、重复性和稳定性进行考察;用平板扫描仪获取23批附子配方颗粒的|ΔG|值(绿色G,|ΔG|=|G_后-G_前|),同时采用LC-MS/MS测定附子配方颗粒中3种生物碱的含量,将|ΔG|与强心成分总含量进行相关性分析。结果 供试品制备方法优选为取附子配方颗粒粉末0.5 g,加10 mL甲醇,300 W、60 kHz超声提取15 min,将上清液全部转移至蒸发皿中,80℃挥干,4 mL 0.13 g/mL的EDTA-2Na溶液洗脱蒸发皿上物质,离心,取上清液,调pH至8.0左右,缓冲溶液稀释3倍。方法学考察表明该方法精密度、重复性和稳定性良好。23批样品的强心成分总含量的差异较大,为127.83~6 928.27 μg/g;|ΔG|的范围为0~12.5,两者的相关系数(r)高达0.96,表明强心成分总含量与|ΔG|高度相关。结论 该方法具有一定的科学性与准确性,可整体性评价附子配方颗粒强心药效。

Objective Based on the similar structure of adrenaline shared by higenamine, salsolinol and coryneine, a photochemical colorimetric sensor based on the displacement reaction of o-diphenol hydroxyl group and alizarin red S-phenylboric acid system was proposed to evaluate the cardiotonic effect of Fuzi (Aconiti Lateralis Radix Praeparata) formula granules as a whole. Methods Taking the response intensity of the sensor as the evaluation index, the preparation conditions of test samples such as ultrasonic extraction time, solid-liquid ratio, extraction solution concentration and EDTA-2Na concentration were optimized; then the precision, repeatability and stability of the method were investigated; The|ΔG|value (G is green,|ΔG|=|G_after-G_before|) of each sample was obtained by response values determination of 23 batches of Fuzi formula granules; at the same time, the contents of three alkaloids in Fuzi formula granules were determined by LC-MS/MS. The correlation between|ΔG|and the total content of cardiac components was analyzed. Results The preparation method of the test article was preferably as follows:take 0.5 g of Fuzi formula granular powder, add 10 mL of methanol, and ultrasonic at 300 W and 60 kHz for 15 min, put the supernatant in an evaporating dish, volatilize it at 80℃, elute the substance on the evaporating dish with 4 mL of 0.13 g/mL EDTA-2Na solution, centrifuge, take the supernatant, adjust the pH to 8.0, and dilute the buffer solution three times; The methodological investigation showed that the method had good precision, repeatability and stability. The total content of cardiac components in 23 batches of samples varied greatly, 127.83-6 928.27 μg/g; The range of|ΔG|was 0-12.5, and the correlation coefficient (r) was as high as 0.96, indicating that the total content of cardiac components was highly correlated with|ΔG|. Conclusion The method is scientific and accurate, and can evaluate the cardiotonic effect of Fuzi formula granules as a whole.

R283.6

四川省中医药管理局科学技术研究专项（2021MS016）；国家自然科学基金青年科学基金项目（82003907）；四川省中医药管理局中医药重点学科建设项目（川中医药函[2020]84号）；四川省重点研发项目（2022YFS0429）