UPLC-MS/MS法同时测定彝族药紫地榆中11个化学成分的含量  

Simultaneous determination of 11 chemical constituents in Yi nationality medicine Geranium strictipes Knuth by UPLC-MS/MS

作　　者：郗仲玟 田宇柔 冯玉 李军山 牛丽颖[1,2,3,4] XI Zhong-wen;TIAN Yu-rou;FENG Yu;LI Jun-shan;NIU Li-ying(Hebei University of Chinese Medicine,Shijiazhuang 050091,China;Hebei Traditional Chinese Medicine Formula Granule Engineering&Technology Innovate Center,Shijiazhuang 050091,China;Quality Evaluation&Standardization Hebei Province Engineering Research Center of Traditional Chinese Medicine,Shijiazhuang 050091,China;TCM Formula Granule Research Center of Hebei Province University,Shijiazhuang 050091,China;Shineway Pharmaceutical Group Company Limited,Shijiazhuang 051430,China)

机构地区：[1]河北中医学院,石家庄050091 [2]河北省中药配方颗粒技术创新中心,石家庄050091 [3]中药材品质评价与标准化河北省工程研究中心,石家庄050091 [4]河北省高校中药配方颗粒应用技术研发中心,石家庄050091 [5]神威药业集团有限公司,石家庄051430

出　　处：《药物分析杂志》2023年第4期573-581,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：中央引导地方科技发展资金项目(206Z2501G);河北省重点研发计划项目(20372502D);云南省重大科技专项计划(202102AA310027)。

摘　　要：目的:采用超高效液相色谱-串联质谱(UPLC-MS/MS)法同时测定彝族药紫地榆中11个化学成分(没食子酸、没食子酸甲酯、儿茶素、短叶苏木酚酸、柯里拉京、老鹳草素、鞣花酸、异槲皮苷、五没食子酰葡萄糖、紫云英苷、齐墩果酸)的含量。方法:采用Shim-pack GIST C_(18)色谱柱(100 mm×2.1 mm, 2.0μm),以乙腈-0.1%乙酸水为流动相进行梯度洗脱,流速为0.4 mL·min^(-1),柱温为30℃,进样量为1μL;采用电喷雾离子源(ESI),以多重反应监测(multiple reaction monitoring, MRM)模式负离子检测。结果:所测11个化学成分在测定浓度范围内线性关系良好,r均>0.999 4;精密度、重复性和稳定性良好,RSD均≤4.6%;平均加样回收率为98.7%~109.7%,RSD≤3.3%。15批样品中没食子酸、没食子酸甲酯、儿茶素、短叶苏木酚酸、柯里拉京、老鹳草素、鞣花酸、异槲皮苷、五没食子酰葡萄糖、紫云英苷、齐墩果酸的含量测定结果为1 084.0~3 533.2、62.4~345.0、206.8~641.2、741.0~1 483.4、2 502.0~4 073.8、15 826.4~68 268.6、0.3~18.1、42.4~128.0、2 349.5~7 670.9、3.9~49.7、1.6~29.6μg·g^(-1)。结论:本方法准确灵敏,稳定性和重复性好,适用于紫地榆的质量评价,为紫地榆的质量控制及临床应用提供参考。Objective:To use an ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the simultaneous determination of the contents of 11 chemical components(gallic acid,methyl gallate,catechin,brervifolincaboxylic acid,corilagin,eraniin,ellagic acid,isoquercitrin,pentagalloyl glucose,astragalin and oleanic acid)in Yi nationality medicine G.strictipes.Methods:The separation was performed on a Shim-pack GIST C_(18)column(100 mm×2.1 mm,2.0μm)with a mobile phase consisting of acetonitrile(A)and 0.1%acetic acid water solution(B)in gradient elution.The flow rate was 0.4 mL·min^(-1),the column temperature was set at 30℃and the injection volume was 1μL.Electrospray ionization(ESI)was used for negative ion detection in multiple reaction monitoring(MRM)mode.Results:The measured 11 chemical components had good linear relationship within the range of measured concentration with correlation coefficients(r)all above 0.9994.The precision,repeatability and stability were good with RSDs≤4.6%.The average recoveries varied between 98.7%and 109.7%with RSDs≤3.3%.The contents of gallic acid,methyl gallate,catechin,brervifolincaboxylic acid,corilagin,eraniin,ellagic acid,isoquercitrin,pentagalloyl glucose,astragalin and oleanic acid in 15 batches of samples were 1084.0-3533.2,62.4-345.0,206.8-641.2,741.0-1483.4,2502.0-4073.8,15826.4-68268.6,0.3-18.1,42.4-128.0,2349.5-7670.9,3.9-49.7 and 1.6-29.6μg·g^(-1),respectively.Conclusion:The method is accurate and sensitive,with good stability and reproducibility,and can be applied to the quality assessment of G.strictipes.It also can provide reference for the quality control and clinical application of G.strictipes used for the quality control and subsequent development and research of the medicinal materials of G.strictipes.

关 键 词：紫地榆 超高效液相色谱-串联质谱 含量测定 质量控制 老鹳草素 短叶苏木酚酸 五没食子酰葡萄糖 

分 类 号：R917[医药卫生—药物分析学]