HPLC-MS/MS法同时测定首荟通便胶囊中8种成份分析  

Hplc-Ms/Ms Method Used for Simultaneous Determination of 8 Components in Shouhui Tongbian Capsule

作　　者：彭艳[1] 陶箭飞 PENG Yan;TAO Jianfei(School of Pharmacy,Nanjing Medical University,Nanjing 211166,China;Department of Pharmacy,Shanghai Yangsi Hospital,Shanghai 200126,China)

机构地区：[1]南京医科大学药学院,南京211166 [2]上海杨思医院药剂科,上海200126

出　　处：《世界中医药》2020年第14期2048-2052,共5页World Chinese Medicine

基　　金：国家自然科学基金面上项目(30300435)。

摘　　要：目的:研究高效液相色谱-串联质谱(HPLC-MS/MS)法同时测定首荟通便胶囊中8种成份的作用。方法:采用HPLC-MS/MS法同时对首荟通便胶囊中8种成份进行分析,采用Agilent ZORBAX C 18色谱柱(250 mm×4.6 mm,5μm),将乙腈(A)-10 mmol/L乙酸铵溶液(B)作为流动相。梯度洗脱(0~1.2 min,5%A;1.2~2 min,5%A→20%A;2~4 min,20%A→40%A;4~8 min,40%A;8~10 min,40%A→95%A;10~17 min,95%A;17~25 min,5%A),设置流速为0.8 mL/min,进样量为5μL。以电喷雾离子源,通过SIM模式,正负离子同时监测方式。结果:何首乌中大黄素、芦荟中芦荟大黄素、决明子中橙黄决明素、枸杞子中枸杞多糖、阿胶中强脯氨酸、人参中人参皂苷、白术中苍术酮、枳实中橙皮苷的线性范围分别为0.04~2.50μg/mL(r=0.9998)、0.034~0.9980μg/mL(r=0.9996)、0.14~20μg/mL(r=0.9994)、0.04~20μg/mL(r=0.9999)、0.004~2μg/mL(r=0.9999)、0.05~2μg/mL(r=0.9996)、0.034~2.5μg/mL(r=0.9993)、0.007~0.2μg/mL(r=0.9995)。本方式的精密度、稳定性及重复性试验的RSD<3%,且平均回收率在97.3~102.7%范围内,RSD均<3%。3种样品中大黄素、芦荟大黄素、橙黄决明素、枸杞多糖、强脯氨酸、人参皂苷、苍术酮、橙皮苷的含量分别为0.491~0.499、1.790~1.802、0.506~0.512、0.681~0.684、0.610~0.614、0.102~0.110、0.056~0.058、0.020~0.022 mg/g。结论:HPLC-MS/MS法可为首荟通便胶囊的质量控制提供指导作用,值得临床推广应用。Objective:To study the simultaneous determination of 8 components in Shouhui tongbian Capsule by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods:A total of 8 components in the Shouhui Tongbian Capsule were analyzed by HPLC-MS/MS method.Agilent ZORBAX C18 column(250 mm×4.6 mm,5 microns)was used.Acetonitrile(A)-10 mmol/L ammonium acetate solution(B)was used as the mobile phase.Gradient elution(0~1.2 min,5%A;1.2~2 min,5%A→20%A;2~4 min,20%A→40%A;4~8 min,40%A;8 min to 10 min,40%A→95%A;10~17 min,95%A;17~25 min,5%A).The flow rate was set as 0.8 mL/min,and the sample volume was 5 mul.To electrospray ion source,through SIM mode,positive and negative ions were simultaneously monitored.Results:Emodin in Radix Polygoni Multiflori,aloe-emodin in Aloe vera L.var,aurantio-obtusin in Semen Cassiae(semen cassiae torae,lycium barbarum polysaccharide in Fructus Lycii the fruit of Chinese wolfberry,strong proline in Colla Corii Asini donkey-hide gelatin,ginsenoside in Radix Ginseng,atractylone in Rhizoma Atractylodis Macrocephalae bighead atractylodes rhizome,and hesperidin in Fructus Aurantii Immaturus were 0.04~2.50μg/mL(r=0.9998),0.034~0.998μg/mL(r=0.9996),0.014~20μg/mL(r=0.9994),0.04~20μg/mL(r=0.9999),0.05~2μg/mL(r=0.9996),0.034~2.5μg/mL(r=0.9993),respectively,0.007~0.2μg/mL(r=0.9995).The RSD of precision,stability and repeatability test of this method was less than 3%,and the average recovery was within the range of 97.3~102.7%,and the RSD was all less than 3%.The contents of emodin,aloe-emodin,aurantio-obtusin,lycium barbarum polysaccharide,strong proline,ginsenoside,atractylone,and hesperidin were 0.491~0.499,1.790~1.802,0.506~0.512,0.681~0.684,0.610~0.614,0.102~0.110,0.056~0.058,0.020~0.022 mg/g,respectively.Conclusion:HPLC-MS/MS method can provide guidance for the quality control of Shouhui tongbian Capsule and is worthy of clinical application.

关 键 词：首荟通便胶囊 高效液相色谱-串联质谱 多成分含量测定 何首乌 芦荟 

分 类 号：R917[医药卫生—药物分析学]