GC-MS法测定麝香保心丸中龙脑、异龙脑、麝香酮、苯甲酸苄酯的含量.docVIP

GC-MS法测定麝香保心丸中龙脑、异龙脑、麝香酮、苯甲酸苄酯的含量 2007年2月 第29卷第2期 中成药 ChineseTlladitionalPatentMedicine February2007 Vo1.29No.2 [质量] GC.MS法测定麝香保心丸中龙脑,异龙脑,麝香酮,苯甲酸苄酯的含量 陈长功,安毅,王新宏h,刘玉敏 (1.上海中医药大学化学教研室,上海201203;2.上海交通大学分析测试中心,上海200030) 关键词:气相色谱质谱法;麝香保心丸;含量测定 摘要:目的:建立麝香保心丸中龙脑,异龙脑,麝香酮,苯甲酸苄酯的GC—MS测定法.方法:以正己烷为溶剂,采用气相色 谱.质谱联用法中选择性离子检测(SIM)方式对麝香保心丸中龙脑,异龙脑,麝香酮,苯甲酸苄酯进行含量测定.DB-5 (0.1m×0.25lnin×30m)石英毛细管柱;80℃～260℃程序升温;选择m/z95为龙脑,异龙脑检测离子,m/z238为麝 香酮的检测离子,m/z212为苯甲酸苄酯检测离子.结果:龙脑,异龙脑,麝香酮,苯甲酸苄酯的线性范围分别为0.020— 20.0I~g/mL(r=0.9993),0.024～24.0~s/mL(r=0.9990),0.029～28.8~g/mL(r=0.9991),0.050～50.0I~g/mL(r :0.9992).平均回收率:龙脑97.00%;异龙脑96.30%;麝香酮96.85%;苯甲酸苄酯98.加%.结论:该方法快速,准 确,有效,可用于麝香保心丸的质量控制. 中图分类号:R927.2文献标识码:A文章编号:1001—1528(20cr7)02-0215-03 Assayofborneol,isoborneol,muscone,benzylbenzoateinShexiangBaoxin Pills CHENChang—gong, ANRui, WANGXin—hong, LIUYu—min (J.CMmico/Department,ShanghaiUniversityofTraditionalChineseMedicine,Shanghai201203,China;2.ChinaNationalAnalyticalCenterof ShanghaiJiaotongUnive~ity,shanghai200030,China) KEYWORDS:GC—MS;ShexiangBaoxinPills;contentdetermination ABSTRACT:AIM:Toestablishthemethodsfordeterminingbomeol,isobomeol,muscone.benzylbenzoatein ShexiangBaoxinPills.METHODS:TurbomassGC—MSinstrumentwasused:theselectiveionwasappliedforde— tectingbomeol,isoborueol,muscone,benzylbenzoate.DB-5capillarycolumn(0.1m×0.25mm×30m).,I1he columRtemperaturewasrosebyprogramfrom80℃to260℃:thequanfiativeionm/z95usedforborueoland isoborneal,m/z238formusone,m/z212forbenzylbenzoate;ShexiangBaoxinPillsweredilutedwithhexane. 砌ULTS:,I1helinearrangesofbomeol,isoborbeol,muscone,benzylbenzoatewerewithin0.020—20.0g/mL (r=0.9993),0.024—24.0g/mL(r=0.9990),0.029—28.8g/mL(r=0.9991),0.050—50.0g/mL (r=0.9992)respectively.,I1heaveragerecoveriesofborueol,isoborbeol,muscone,benzylbenzoatewere97. 00%,96.30%,96.85%,98.20%,respectively.CONCLUSION:Themethodissimpleaccurateandhighly sensitiveandsuitableforShexiangBaoxinPills. 麝香保心丸由麝香,冰片,人参,蟾酥等中药组 成…,含有多种挥发性成分,指标性成分含量低且 各种成分的含量差别较大,文献报道用气相色谱法 在不同条件下测定冰片,麝香酮的含量].本实 验采用了气相色谱质谱联用