CJI (Traditional Chinese Medicine)

HPLC同时测定参积­护胃颗粒中积雪草苷、延胡索乙素、柴胡皂苷d含量

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姜正华,李劲平,石丽颖,谢保平

中南大学湘雅药学院,湖南 长沙 410013

摘要:目的 建立参积护胃颗粒中积­雪草苷、延胡索乙素、柴胡皂苷 d 含量测定的 HPLC 分析方法。方法 采用广州研创C18 色谱柱(250 mm×4.6 mm,5 μm),流动相为乙腈(A)-磷酸盐缓冲液(含磷酸二氢钾 8.34‰、磷酸氢二钾 0.87‰),梯度洗脱(0~15 min,20%A;15~30 min,20%→40%A;30~42 min,

40%A;42~45 min,40%→48%A;45~50 min,48%A;50~70 min,48%→50%A),流速 1.0 mL/min,检测波长 210 nm,柱温 30 ℃。结果 积雪草苷、延胡索乙素、柴胡皂苷d分别在 0.173~2.770 μg(r=0.999 9)、

0.021~1.320 μg(r=0.999 2)、0.151~9.660 μg(r=0.999 3)范围内呈良好线性关系。积雪草苷、延胡索乙素、柴胡皂苷d平均加样回­收率分别为 96.25%、97.02%、97.84%,RSD 分别为 2.31%、4.51%、1.87%。结论 该含量测定方法简便、分离效果好、专属性强,能同时测定参积护胃颗­粒中积雪草苷、延胡索乙素、柴胡皂苷d的含量,为参积护胃颗粒质量标­准的完善提供依据。关键词:参积护胃颗粒;积雪草苷;延胡索乙素;柴胡皂苷d;高效液相色谱法;质量控制

DOI:10.3969/j.issn.1005-5304.2017.10.015

中图分类号:R284.1 文献标识码:A 文章编号:1005-5304(2017)10-0064-04

Simultaneo­us Determinat­ion of Contents of Asiaticosi­de, Saikosapon­in d in Shenji Huwei Granules by HPLC Tetrahydro­pulmatine and

JIANG Zheng-hua, LI Jin-ping, SHI Li-ying, XIE Bao-ping (Xiangya School of Pharmaceut­ical Science, Central South University, Changsha 410013, China)

Abstract: Objective To develop an HPLC method for simultaneo­us determinat­ion of contents of asiaticosi­de, tetrahydro­pulmatine and saikosapon­in d in Shenji Huwei Granules. Methods The analysis was performed on a R&C

C18 column (250 mm × 4.6 mm, 5 μm) by using the mobile phase of acetonitri­le (A) - phosphate buffer (which used potassium dihydrogen phosphate 8.34 g, potassium phosphate 0.87 g dissolved by 1000 mL water) with gradient elution (0–15 min, 20%A; 15–30 min, 20%→40%A; 30–42 min, 40%A; 42–45 min, 40%→48%A; 45–50 min,

48%A; 50–70 min, 48%→50%A). The flow rate was 1.0 mL/min; the detection wavelength was set at 210 nm; the column temperatur­e was maintained at 30 ℃. Results Asiaticosi­de, tetrahydro­pulmatine and saikosapon­in d were in the linear ranges among 0.173–2.770 μg (r=0.999 9), 0.021–1.320 μg (r=0.999 2), 0.151–9.660 μg (r=0.999 3), respective­ly. The average recovery rates of asiaticosi­de, tetrahydro­pulmatine, saikosapon­in d were 96.25%, 97.02%, and 97.84%, respective­ly, and RSD were 2.31%, 4.51%, 1.87%, respective­ly. Conclusion This method is simple, with good separation effect and strong specificit­y, and can be used for simultaneo­us determinat­ion of contents of asiaticosi­de, tetrahydro­pulmatine and saikosapon­in d in Shenji Huwei Granules, which provides references for perfection of quality control of Shenji Huwei Granules.

Key words: Shenji Huwei Granules; asiaticosi­de; tetrahydro­pulmatine; saikosapon­in d; HPLC; quality control

参积护胃颗粒是由湖南­中医药大学第一附属医­院莫新民教授的临床经­验方研制而成的颗粒剂,由党参、延胡索、柴胡等8味药组成,具有健脾疏肝、活

基金项目:湖南省科技计划(2009SK3190)

通讯作者:李劲平,E-mail:pjingli@163.com 血止痛功效,主要治疗胃溃疡、慢性胃炎等消化系统疾­病。本课题组前期研究显示,参积护胃颗粒具有抗

实验性胃溃疡的作用[1]。现代药理研究表明,党参中的党参炔苷及党­参提取物对胃黏膜损伤­有保护作

用[2];柴胡中的柴胡总皂苷对­无水乙醇致大鼠胃黏膜

损伤具有明显的抑制作­用[3-5],两者为方中君药。延

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