摘要
目的建立HPLC法测定保元汤颗粒中毛蕊异黄酮葡萄糖苷的含量。方法根据《中国药典》规定的方法,并加以优化,以AgilentEclipseplus(5μm,4.6mm×250mm)为色谱柱,以乙腈(A)-0.2%甲酸溶液(B)为流动相,梯度洗脱(0~20min,15%~40%A;20~25min,40%A),流速1.0mL/min,柱温25℃,检测波长260nm。结果经方法学验证,毛蕊异黄酮葡萄糖苷在25.23~504.5ng(R2=0.9995)范围内线性关系良好,该检测方法专属性较好,阴性无干扰,精密度RSD为0.26%,重复性RSD为3.98%,中间精密度RSD为3.12%,加样回收率为93.63%(RSD为3.98%),溶液稳定性在8h以内可保持稳定(RSD为1.47%),该方法耐用性较好。经测定,甘草中毛蕊异黄酮葡萄糖苷含量为0.0045~0.0161%,保元汤颗粒(含有辅料,6g/袋)中为87.98~97.46μg·g-1。结论本研究所建立的方法简便,结果准确可靠,适用于保元汤颗粒中毛蕊异黄酮葡萄糖苷的测定,为建立保元汤质量标准提供依据。此外,本研究首次对甘草中毛蕊异黄酮葡萄糖苷进行了鉴别及含量测定,为甘草及其制剂质量标准深入研究奠定基础。
Objective: To establish a HPLC method for the determination of calycosin isoflavone glucoside in Baoyuantang granules. Methods: According to the method specified in the Chinese Pharmacopoeia, Agilent Eclipse plus(5μm, 4.6 mm×250 mm) was taken as chromatographic column and acetonitrile(A)-0.2% formic acid solution(B) as mobile phase, with gradient elution(0~20 min, 15%~40%A;20~25 min, 40%A), flow rate 1.0 mL/min, column temperature 25℃, and detection wavelength 260 nm. Results: The method showed that calycosin isoflavone glucoside had a good linear relationship in the range of 25.23 to 504.5 ng(R2=0.9995). The detection method had good specificity and no interference. The precision RSD was 0.26% and the reproducible RSD was 3.98%, and the intermediate precision RSD is 3.12%. The sample recovery rate was 93.63%(RSD is 3.98%), and the solution stability could be kept stable within 8 h(RSD is 1.47%). The method had better durability. The content of calycosin isoflavone glucoside in the licorice was determined to be 0.0045-0.0161%, and that in the Baoyuantang granules(containing excipients, 6 g/bag) was 87.98~97.46μg·g-1. Conclusion: The method established in this study is simple, accurate and reliable and suitable for the determination of calycosin isoflavone glucoside in the Baoyuantang granules, and provides a basis for establishing the quality standard of Baoyuantang. In addition, the study was the first to identify and determine the content of calycosin isoflavone glucosides in licorice and lay a foundation for further research on the quality standards of licorice and its preparations.
作者
袁玲玲
钱如贵
丁丽娜
李心锋
YUAN Ling-ling;QIAN Ru-gui;DING Li-na;LI Xin-feng(Kunming Bangyu Pharmaceutical Co., Ltd., Kunming 650211, China)
出处
《云南中医中药杂志》
2019年第8期69-75,共7页
Yunnan Journal of Traditional Chinese Medicine and Materia Medica