UFLC-MS/MS法同时测定栀子厚朴汤中10个成分的含量  

Simultaneous determination of ten components in Zhizi Houpo decoction by UFLC-MS/MS

作　　者：朱鹤云 王开鼎 史健艺 张葆祺 赵宏宇 冯波 关皎 ZHU He-yun;WANG Kai-ding;SHI Jian-yi;ZHANG Bao-qi;ZHAO Hong-yu;FENG Bo;GUAN Jiao(School of Pharmacy,Jilin Medical University,Jilin 132013,China)

机构地区：[1]吉林医药学院药学院,吉林132013

出　　处：《药物分析杂志》2020年第10期1751-1759,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金项目(81703683,81773692);吉林省教育厅项目(JJKH20191071KJ);吉林省中医药管理局项目(2017098,2018124,2017250);吉林省卫生计生委项目(2017Q048);国家级大学生创新创业项目(201913706014,201813706005)。

摘　　要：目的:建立超快速液相色谱-串联质谱法同时测定栀子厚朴汤中10个成分(京尼平苷、京尼平龙胆双糖苷、和厚朴酚、厚朴酚、异柚皮苷、柚皮苷、橙皮苷、新橙皮苷、柚皮素和橙皮素)的含量。方法:采用Shim-Pack XR-ODS色谱柱(75 mm×3.0 mm,2.2μm),流动相为0.1%甲酸水溶液(A)-乙腈(B),梯度洗脱(0~10 min,10%B→30%B;10~12 min,30%B→60%B;12~18 min,60%B→85%B),平衡时间为5min,流速为0.5 mL·min-1,柱温为30℃,进样量为5μL;质谱采用3200 QTRAP三重四极杆串联质谱仪,离子源为电喷雾电离源(ESI源),检测方式为负离子检测,扫描模式为多反应检测(MRM)。结果:京尼平苷、京尼平龙胆双糖苷、和厚朴酚、厚朴酚、异柚皮苷、柚皮苷、橙皮苷、新橙皮苷、柚皮素和橙皮素质量浓度分别在1~40μg·mL-1(r=0.999 6)、0.2~8μg·mL-1(r=0.999 7)、0.1~4μg·mL-1(r=0.999 3)、0.1~4μg·mL-1(r=0.999 7)、0.2~8μg·mL-1(r=0.999 5)、1~40μg·mL-1(r=0.999 7)、0.2~8μg·mL-1(r=0.998 5)、1~40μg·m L-1(r=0.999 7)、0.1~4μg·m L-1(r=0.999 2)和0.02~0.8μg·m L-1(r=0.999 4)范围内与峰面积呈良好的线性关系;平均回收率(n=9)分别为98.0%、98.5%、96.9%、98.8%、98.4%、99.3%、99.4%、98.7%、98.9%和97.9%。6批样品中上述10个成分的含量范围分别为京尼平苷4.51%~4.83%,京尼平龙胆双糖苷0.805%~0.841%,和厚朴酚0.125%~0.134%,厚朴酚0.133%~0.144%,异柚皮苷0.403%~0.435%,柚皮苷5.54%~5.84%,橙皮苷0.210%~0.222%,新橙皮苷3.98%~4.30%,柚皮素0.059 2%~0.066 0%,橙皮素0.021 3%~0.022 3%。结论:本方法准确灵敏,稳定性和重复性好,可用于栀子厚朴汤的质量控制。Objective:To establish an ultra-fast liquid chromatography with tandem mass spectrometry(UFLCMS/MS) method for simultaneous determination of geniposide,genipin gentiobioside,honokiol,magnolol,isonaringin,naringin,hesperidin,neohesperidin,naringenin and hesperetin in Zhizi Houpo decoction. Methods:Chromatographic separation was performed on a Shim-Pack XR-ODS column(75 mm×3.0 mm,2.2 μm). The mobile phase consisted of 0.1% formic acid(A) and acetonitrile(B) at a flow rate of 0.5 mL·min-1. The ten analytes were determined with gradient elution(0-10 min,10%B→30%B;10-12 min,30%B→60%B;12-18 min,60%B→85%B),and the equilibration time was 5 min. The column temperature was maintained at 30 ℃,and the injection volume was 5 μL. Detection was performed on 3200 QTRAP mass spectrometry equipped with electrospray ionization source in negative ionization mode. Quantification was performed using multiple reactions monitoring(MRM) mode. Results:The linear ranges of geniposide,genipin gentiobioside,honokiol,magnolol,isonaringin,naringin,hesperidin,neohesperidin,naringenin and hesperetin were 1-40 μg·mL-1(r=0.999 6),0.2-8 μg·mL-1(r=0.999 7),0.1-4 μg·mL-1(r=0.999 3),0.1-4 μg·mL-1(r=0.999 7),0.2-8 μg·mL-1(r=0.9995),1-40 μg·mL-1(r=0.999 7),0.2-8 μg·mL-1(r=0.998 5),1-40 μg·mL-1(r=0.999 7),0.1-4 μg·mL-1(r=0.999 2) and 0.02-0.8 μg·mL-1(r=0.999 4),respectively. The average recoveries(n=9) of the above-mentioned ten components were 98.0%,98.5 %,96.9%,98.8%,98.4%,99.3%,99.4%,98.7%,98.9% and 97.9%,respectively. The content ranges of ten components in six batches were 4.51%-4.83% for geniposide,0.805%-0.841% for genipin gentiobioside,0.125%-0.134% for honokiol,0.133%-0.144% for magnolol,0.403%-0.435% for isonaringin,5.54%-5.84% for naringin,0.210%-0.222% for hesperidin,3.98%-4.30% for neohesperidin,0.059 2%-0.066 0% for naringenin and 0.021 3%-0.022 3% for hesperetin. Conclusion:The established method is accurate,stable and reproducible,and can provide a research method for the quality control of Zhizi Houpo deco

关 键 词：栀子厚朴汤 栀子 厚朴 枳实 京尼平苷 京尼平龙胆双糖苷 和厚朴酚 厚朴酚 异柚皮苷 柚皮苷 橙皮苷 新橙皮苷 柚皮素 橙皮素 环烯醚萜苷类化合物 木脂素类化合物 黄酮类化合物 超快速液相色谱-串联质谱法 

分 类 号：R917[医药卫生—药物分析学]