Page 71 - 2019年10月第30卷第20期

·中药与民族药·

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 Δ

＊
温子帅 ，李新蕊，木盼盼，宋军娜，张彦昭，郑玉光，严玉平，马东来（河北中医学院药学院，石家庄 050200）
#
中图分类号 R284.1 文献标志码 A 文章编号 1001-0408（2019）20-2802-06
DOI 10.6039/j.issn.1001-0408.2019.20.13

摘 要 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1.0 mL/min，柱温为30 ℃，漂移管温
度为90 ℃，载气流速为2.9 L/min，进样体积为20 μL。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SPSS
22.0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1.03～6.18 μg/mL（r＝0.999 7）、1.05～6.30 μg/mL（r＝0.999 8）；定量限
分别为0.171、0.174 μg/mL，检测限分别为0.052、0.053 μg/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。
关键词 酸枣仁；斯皮诺素；酸枣仁皂苷A；高效液相色谱-蒸发光散射检测法；含量测定；中药质量常数；质量等级

Contents of Determination Spinosin and Jujuboside A in the Seads of Ziziphus jujuba and Its Quality
Grading Standard
WEN Zishuai，LI Xinrui，MU Panpan，SONG Junna，ZHANG Yanzhao，ZHENG Yuguang，YAN Yuping，MA
Donglai（College of Pharmacy，Hebei University of TCM，Shijiazhuang 050200，China）

ABSTRACT 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.
KEYWORDS The seads of Ziziphus jujuba；Spinosin，Jujuboside A；HPLC-ELSD；Content determination；Quality constant；
Quality level
酸枣仁为鼠李科植物酸枣[Ziziphus jujuba Mill. var.
Δ 基金项目：国家自然科学基金资助项目（No.81803762）；国家中
药标准化项目（No.ZYBZH-Y-ZY-45）；河北省中医药管理局科研计划 spinosa（Bunge）Hu ex H. F. Chou]的干燥成熟种子，始载
项 目（No.2018105）；河 北 省 高 等 学 校 科 学 技 术 研 究 项 目（No. 于《神农本草经》，列为上品，其味甘、酸，性平，归肝、胆、
QN2018065） [1]
心经，具有宁心安神、养心补肝、敛汗、生津的功效 。现
＊硕士研究生。研究方向：中药资源与鉴定。E-mail：wenzish-
代药理研究表明，酸枣仁具有降血压、抗焦虑、抗心肌缺
uai802@163.com
[2]
血、治疗神经衰弱等作用 ，为中医临床常用药，主产于
# 通信作者：副教授，硕士生导师，博士。研究方向：中药质量分
[3]
析与控制。电话：0311-89926350。E-mail：mdl_hebei@aliyun.com 河北、山东、辽宁、陕西等地 。酸枣仁为临床治疗失眠
·2802 · China Pharmacy 2019 Vol. 30 No. 20 中国药房 2019年第30卷第20期