Wang Xiaoli, Liu Xiao, Zhu Tingting, Cai Baochang
School of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210023, China; Engineering Center of State Ministry of Education for Standardization of Chinese Medicine Processing, Nanjing University of Chinese Medicine, Nanjing 210023, China; Nanjing Haichang Chinese Medicine Group Corporation, Nanjing 210061, China.
School of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210023, China.
J Anal Methods Chem. 2016;2016:1435106. doi: 10.1155/2016/1435106. Epub 2016 May 26.
The aim of this study is to develop an ultrahigh performance liquid chromatography method coupled with triple quadrupole mass spectrometry for simultaneous determination of tetrandrine, fangchinoline, atractylenolide I, atractylenolide III, calycosin-7-O-β-D-glucoside, glycyrrhizin, liquiritin, isoliquiritin, liquiritigenin, and isoliquiritigenin in Fangji Huangqi Tang (FHT). The chromatographic separation was performed on a reversed-C18 column, eluted with a mixture of 0.1% acetic acid and acetonitrile at 0.4 mL/min. The separation of these ten compounds was achieved by linear gradient elution. The method was strictly validated with respect to specificity, precision, accuracy, and repeatability. All the compounds showed good linearities (r ≥ 0.999). The LOQs of the ten components were 0.36, 0.18, 0.09, 0.43, 0.02, 1.89, 0.26, 0.18, 0.61, and 0.48 ng/mL for tetrandrine, fangchinoline, atractylenolide I, atractylenolide III, calycosin-7-O-β-D-glucoside, glycyrrhizin, liquiritin, isoliquiritin, liquiritigenin, and isoliquiritigenin, respectively. The LODs of the ten components were 0.11, 0.05, 0.03, 0.13, 0.01, 0.57, 0.08, 0.05, 0.18, and 0.14 ng/mL for tetrandrine, fangchinoline, atractylenolide I, atractylenolide III, calycosin-7-O-β-D-glucoside, glycyrrhizin, liquiritin, isoliquiritin, liquiritigenin, and isoliquiritigenin, respectively. The method was proven to be specific and reliable, which would provide a meaningful basis for the quality control and evaluation of FHT during its clinical application.
本研究旨在开发一种超高效液相色谱法结合三重四极杆质谱法，用于同时测定防己黄芪汤（FHT）中的粉防己碱、防己诺林碱、白术内酯I、白术内酯III、毛蕊异黄酮葡萄糖苷、甘草酸、甘草苷、异甘草苷、甘草素和异甘草素。色谱分离在反相C18柱上进行，以0.1%乙酸和乙腈的混合物以0.4 mL/min的流速洗脱。通过线性梯度洗脱实现这十种化合物的分离。该方法在特异性、精密度、准确度和重复性方面进行了严格验证。所有化合物均表现出良好的线性关系（r≥0.999）。粉防己碱、防己诺林碱、白术内酯I、白术内酯III、毛蕊异黄酮葡萄糖苷、甘草酸、甘草苷、异甘草苷、甘草素和异甘草素这十种成分的定量限分别为0.36、0.18、0.09、0.43、0.02、1.89、0.26、0.18、0.61和0.48 ng/mL。这十种成分的检测限分别为0.11、0.05、0.03、0.13、0.01、0.57、0.08、0.05、0.18和0.14 ng/mL。该方法被证明具有特异性和可靠性，可为FHT临床应用中的质量控制和评价提供有意义的依据。
