酸枣仁中斯皮诺素、酸枣仁皂苷A含量测定及其质量等级划分标准研究

Contents of Determination Spinosin and Jujuboside A in the Seads of Ziziphus jujuba and Its Quality Grading Standard

目的:建立同时测定酸枣仁中斯皮诺素、酸枣仁皂苷A含量的方法,并进行质量等级划分。方法:采用高效液相色谱-蒸发光散射检测法测定含量。色谱柱为Inertsil ODS-SP,流动相为乙腈-水(梯度洗脱),流速为1.0mL/min,柱温为30℃,漂移管温度为90℃,载气流速为2.9L/min,进样体积为20μL。以药材样品厚度、宽度、长度、百粒质量为指标,考察其外观性状;采用SPSS22.0软件分析样品中斯皮诺素、酸枣仁皂苷A含量及其外观性状与中药质量常数的相关性,并建立该药材的质量等级划分标准。结果:斯皮诺素、酸枣仁皂苷A的质量浓度线性范围分别为1.03~6.18μg/mL(r=0.9997)、1.05~6.30μg/mL(r=0.9998);定量限分别为0.171、0.174μg/mL,检测限分别为0.052、0.053μg/mL;精密度、稳定性、重复性试验的RSD均小于2%;加样回收率分别为99.01%~102.97%(RSD=1.39%,n=6)、97.94%~101.03%(RSD=1.13%,n=6)。相关性分析结果显示,药材长度、宽度、百粒质量、斯皮诺素含量、酸枣仁皂苷A含量均与其中药质量常数呈正相关。质量等级划分结果显示,30批样品中S1~S4、S7~S12为一等品;S5、S6、S13~S17、S20~S30为二等品;S18、S19为三等品。结论:所建含量测定方法操作简单,精密度、准确度、稳定性均较好,可用于同时测定酸枣仁中斯皮诺素、酸枣仁皂苷A的含量;所建酸枣仁质量等级划分标准可用于综合评价该药材质量。

OBJECTIVE:To establish a method for simultaneous determination of spinosin and jujuboside A in the seads of Ziziphus jujuba,and to investigate its quality grading standard.METHODS:HPLC-ELSD method was adopted.The separation was carried out on Inertsil ODS-SP column with mobile phase consisted of acetonitrile-water(gradient elution)at the flow rate of 1.0 mL/min.The column temperature was 30 ℃,the temperature of drift tube was 90 ℃,the flow of carrier gas was 2.9 L/min and injection volume was 20 μL.The thickness,width,length and 100-grain quality of the medicinal materials were used as indicators to investigate the appearance traits.SPSS 22.0 software was used to analyze the correlation of the contents of spinosin and jujuboside A,its appearance traits with the quality constant of TCM,and establish a quality classification standard for the seads of Z. jujuba.RESULTS:The linear range of spinosin and jujuboside A were 1.03-6.18 μg/mL(r=0.999 7),1.05-6.30 μg/mL(r=0.999 8);the limits of quantitation were 0.171,0.174 μg/mL,respectively;the limits of detection were 0.052,0.053 μg/mL,respectively. RSDs of precision,stability and reproducibility tests were all lower 2%.The recoveries were 99.01%-102.97%(RSD=1.39%, n=6),97.94%-101.03%(RSD=1.13%,n=6),respectively.Correlation analysis results showed that the length,width, 100-grain quality spinosin content and jujuboside A content of the medicinal materials were positively correlated with the quality constant of TCM.The results of quality classification for 30 batches of medicinal materials showed that S1-S4 and S7-S12 were first-class products;S5,S6,S13-S17 and S20-S30 were second-class products;S18 and S19 were third-class products. CONCLUSIONS:Established content determination method is simple,precision,accurate and stable,and can be used for simultaneous determination of spinosin and jujuboside A in the seads of Z.jujuba.Established quality grading standard of the seads of Z.jujuba can be used to evaluate the quality.