UPLC-Q-Orbitrap高分辨质谱定量分析风寒感冒颗粒中的11个成分  

Simultaneous determination of 11 components in Fenghan Ganmao granules by UPLC-Q-Orbitrap high-resolution mass spectrometry

作　　者：张恒斌 王亮 ZHANG Heng—bin;WANG Liang(Linyi Institute for Food and Drug Control,Linyi 276001,China)

机构地区：[1]临沂市检验检测中心

出　　处：《药物分析杂志》2019年第10期1828-1835,共8页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立UPLC-Q-Orbitrap高分辨质谱同时测定风寒感冒颗粒中盐酸麻黄碱、苦杏仁苷、葛根素、升麻素苷、甘草苷、橙皮苷、5-O-甲基维斯阿米醇苷、桂皮醛、桔梗皂苷D、欧前胡素、甘草酸铵含量的方法,为风寒感冒颗粒的质量评价提供参考。方法:采用Thermo Fisher Scientific Hypersil GOLD aQ C18色谱柱(100 mm×2.1 mm,2.7μm),以甲醇-0.1%甲酸水溶液为流动相,梯度洗脱,流速300 mL·min^-1;电喷雾正负离子源同时检测,Full MS/dd-MS2扫描模式,通过比较样品与对照品的色谱保留时间、高分辨一级质谱、色谱峰面积,同时进行11个成分的定量测定。结果:11个成分的线性范围为0.5~200 ng·mL^-1,相关系数(r)均不低于0.998,回收率为90%~110%,RSD为1.1%~2.0%;7批样品中盐酸麻黄碱、苦杏仁苷、葛根素、升麻素苷、甘草苷、橙皮苷、5-O-甲基维斯阿米醇苷、桂皮醛、桔梗皂苷D、欧前胡素、甘草酸铵含量范围分别为26.25~301.25、611.25~1550、157.5~1 850、0~220.0、8.75~140、105.0~451.25、15.0~118.75、0~210、10.0~40.0、12.5~41.25、31.25~302.5μg·g^-1,含量差别明显。结论:该法快速简便,高通量,选择性好,灵敏度高,能为风寒感冒颗粒的质量控制提供依据。Objective:To establish an UPLC-Q-Orbitrap high resolution mass spectrometry method for the simultaneous determination of ephedrine hydrochloride,amygdalin,puerarin,prim-O-glucosylcimifugin,liquiritin,hesperidin,5-O-methylvisammioside,cinnamaldehyde,platycodin D,imperatorin and ammonium glycyrrhizinate in Fenghan Ganmao granules,so as to provide reference for quality evaluation of Fenghan Ganmao granules. Methods:Thermo Fisher Hypersil GOLD aQ C18 column(100 mm×2.1 mm,2.7 μm)was adopted,the mobile phase consisted of methanol-0.1% formic acid aqueous solution with gradient elution at a flow rate of 300 μL·min^-1. Simultaneous detection with ESI+ and ESI-and full MS/dd-MS2 scanning mode were used. 11 components were determined by comparing the chromatographic retention time,high-resolution primary mass spectrometry and chromatographic peak area of the sample and the reference. Results:The linear ranges of 11 components were 0.5 to 200 ng·mL^-1,the correlation coefficients(r)were above 0.998,the recovery rates were 90% to 110% with RSDs between 1.1% to 2.0%. In 7 batches of samples,the contents of ephedrine hydrochloride,amygdalin,puerarin,prim-O-glucosylcimifugin,liquiritin,hesperidin,5-O-methylvisammioside,cinnamaldehyde,platycodin D,imperatorin and ammonium glycyrrhizinate were 26.25-301.25,611.25^-1550,157.5^-1 850,0-220.0,8.75^-140,105.0-451.25,15.0^-118.75,0-210,10.0-40.0,12.5-41.25 and 31.25-302.5 μg·g^-1,respectively,which varied significantly. Conclusion:With high flux,good selectivity and high sensitivity,the method is quick and simple,which can provide evidence for quality control of Fenghan Ganmao granules.

关 键 词：超高效液相色谱 四极杆-静电场轨道阱 高分辨质谱 风寒感冒颗粒 盐酸麻黄碱 苦杏仁苷 葛根素 升麻素苷 甘草苷 橙皮苷 5-O-甲基维斯阿米醇苷 桂皮醛 桔梗皂苷D 欧前胡素 甘草酸铵 定量分析 

分 类 号：R917[医药卫生—药物分析学]