Yang Wei, He Shiyong, Xiao Nan, Qiao Yanling, Sui Hua, Liang Lina, Chen Jing, Li Weiling, Zhang Lin
Affiliated Cancer Hospital of Zhengzhou University, Department of Pharmacy, Zhengzhou 450000, China.
Dalian Medical University, Academy of Integrative Medicine, Dalian 116044, China.
J AOAC Int. 2018 Jul 20. doi: 10.5740/jaoacint.17-0469.
The herb pair has appeared in classical prescriptions and has usually been used for the treatment of cancer and inflammatory conditions. For quality control of this herb pair, a rapid and reliable HPLC-quadrupole-time-of-flight(Q-TOF)-MS method was used for the simultaneous determination of alpinetin, apigenin-7-O-β-D-glucopyranoside, scutellarein, apigenin, quercetin-3-O-β-D-glucopyranoside, wogonoside, quercetin, amentoflavone, wogonin, chrysin, luteolin, rutin, naringenin, baicalein, and baicalin in the herb pair. LC-MS analysis was performed on a Shimadzu HPLC 20ADXR LC system in-line with an AB-SCIEX 5600 Triple TOF mass spectrometer. The calibration curves showed good linearity in a relatively wide concentration range ( >0.996). The LOD and LOQ were less than 20 and 68 ng/mL, respectively. The relative standard deviation (RSD) values of intraday and inter-day precision were <3.31% for all the analytes. The recoveries of the method were in the range of 94.6-106.0%, with RSD <4.72%. The RSD values of peak areas in the stability study were not more than 4.28% for all analytes within 2 days. These results revealed that the method exhibited good sensitivity, precision, accuracy, and stability. This method could be applied to the quantitative determination of 15 flavonoids in the herb pair. () The established method of HPLC-Q-TOF-MS is simple, fast, sensitive, and reliable. () 15 Flavonoids in the herb pair were simultaneous determined.
这味药对已出现在经典方剂中,通常用于治疗癌症和炎症性疾病。为了对这味药对进行质量控制,采用了一种快速可靠的高效液相色谱-四极杆-飞行时间(Q-TOF)-质谱法,同时测定该药对中的山姜素、芹菜素-7-O-β-D-葡萄糖苷、野黄芩素、芹菜素、槲皮素-3-O-β-D-葡萄糖苷、汉黄芩苷、槲皮素、穗花杉双黄酮、汉黄芩素、白杨素、木犀草素、芦丁、柚皮素、黄芩苷元和黄芩苷。液相色谱-质谱分析在一台与AB-SCIEX 5600 Triple TOF质谱仪联用的岛津HPLC 20ADXR液相色谱系统上进行。校准曲线在相对较宽的浓度范围内显示出良好的线性(>0.996)。检测限和定量限分别小于20 ng/mL和68 ng/mL。所有分析物日内和日间精密度的相对标准偏差(RSD)值均<3.31%。该方法的回收率在94.6 - 106.0%范围内,RSD<4.72%。稳定性研究中所有分析物在2天内峰面积的RSD值不超过4.28%。这些结果表明该方法具有良好的灵敏度、精密度、准确度和稳定性。该方法可用于定量测定该药对中的15种黄酮类化合物。()所建立的高效液相色谱-四极杆-飞行时间-质谱法简单、快速、灵敏且可靠。()同时测定了该药对中的15种黄酮类化合物。