反相高效液相色谱法测定大青叶中邻氨基苯甲酸与丁香酸的含量王文清

·药品质量控制·＊王文清,张　飞,方建国,李园园,汪秋兰,汤　杰(,　430030)[　]　　建立测定大青叶中邻氨基苯甲酸和丁香酸含量的反相高效液相色谱法。　固定相:LichrosorbC18色谱柱(4.6mm×150mm,5μm);流动相:乙腈-水-磷酸(18∶82∶0.3);检测波长:272nm;流速:0.8mL·min-1;柱温:30℃;进样体积:10μL。　邻氨基苯甲酸、丁香酸分别在12.7～127.0和5.10～51.0μg·mL-1浓度范围内线性关系良好;邻氨基苯甲酸的平均回收率为98.7%(RSD=1.0%);丁香酸的平均回收率为99.0%(RSD=1.2%)。　该方法灵敏、快速,准确可靠。[]　大青叶;邻氨基苯甲酸;丁香酸;反相高效液相色谱法[]　R927.2;R286　　　[]　A　　　[]　1004-0781(2006)05-0456-02DeterminationofAnthranilicAcidandSyringicAcidinFoliumIsatidisbyRP-HPLCWANGWen-qing,ZHANGFei,FANGJian-guo,LIYuan-yuan,WANGQiu-lan,TANGJie(DepartmentofPharmacy,TongjiHospitalAffiliatedwiththeTongjiMedicalCollege,HuazhongUniversityofScienceandTechnology,Wuhan430030,China)ABSTRACT　Objective　ToestablishaRP-HPLCmethodtodeterminethecontentsofanthranilicacidandsyringicacidinFoliumIsatidis.　Methods　ChromatographywascarriedoutonaLichrosorbC18column(4.6mm×150mm,5μm);mobilephase:acetonitrile-water-phosphoricacid(18∶82∶0.3);flowrate:0.8mL·min-1;columntemperature:30℃,samplevolume:10μL;andthedetectionwavelengthwas272nm.　Results　Agoodlinearityofanthranilicacidwasobtainedwithin12.7-127.0μg·mL-1andsyringicacidwaswithin5.10-51.0μg·mL-1.Theaveragerecoveriesofanthranilicacidwas98.7%(RSD=1.0%);andsyringicacidwas99.0%(RSD=1.2%),respectively.　Conclusion　Themethodissensitive,rapid,andaccurate.KEYWORDS　FoliumIsatidis;Anthranilicacid;Syringicacid;RP-HPLC　　IsatisIndigo-ticaFort.,,、。,、、、[1]。。[2,3]。。、,。1　　Agilent1100,7725i[]　2005-05-12　　　[]　2005-06-20[]　＊(:39800193)[]　(1969-),,,,,。:027-83649095。,;UV-265FW();AUW220D。,,。(:20020510,,99.3%),(:S6881-5G,,Sigma),(,IsatisIndigoticaFort.)。2　　2.1　色谱条件　:LichrosorbC18(4.6mm×150mm,5μm);:--(18∶82∶0.3);:0.8mL·min-1;:272nm;:30℃;:10μL。2.2　对照品溶液的制备　,,0.05mg0.02mg,。·456·HeraldofMedicineVol.25No.5May20062.3　供试品溶液的制备　3.0g,,,60mL,8h,,,,10mL,,,,。2.4　线性关系考察　25.4mg,10.2mg,,100mL,。0.5,1.0,2.0,3.0,4.0,5.0mL10mL,,。10μL,。12.7～127.0μg·mL-1Y=80.574X-1.698,r=0.9998(n=6);5.10～51.0μg·mL-1Y=25.043X-1.1041,r=0.9999(n=6)。2.5　精密度试验　3.0mL50mL,,。6,10μL,RSD0.81%0.93%。2.6　稳定性试验　,0,2,4,6,8h,,RSD0.62%0.78%。8h。2.7　重复性试验　5,3.0g,,“2.3”,,RSD1.54%1.27%,。2.8　回收率试验　91.5g,2.0,3.0,4.0mL。“2.3”,3:99.4%(RSD=0.7%),98.2%(RSD=1.3%),98.6%(RSD=1.1%);:98.1%(RSD=1.0%),99.8%(RSD=1.2%),99.0%(RSD=1.4%)。2.9　样品的含量测定　“2.3”,,0.052mg·g-1,0.027mg·g-1(n=3)。3　　。、、。[][1]　　,.[J].中草药,2000,31(9):664-665.[2]　WuXY,QinGW,ShengZY,etal.Chemicalconstituentsofisatisindigotical[J].PlantaMed,1997,63(33):55-57.[3]　FangJG,LiuYH,WangWQ,etal.AntiendotoxiceffectofO-AminobenzoicacidfromRadixIsatiais[J].中国药理学报,2005,26(5):1025-1028.＊熊学敏1,曹　珏2,张晓辉1,吉刚峰3,朱建平3,陈　乐1,孙　磊4(1.,　330077;2.,　330006;3.2004,　330006;4.,　330006)[　]　　建立金边瑞香滴鼻剂中瑞香素的鉴别及含量测定方法。　采用高效液相色谱法,固定相:DiamonsilTMC18色谱柱(4.6mm×250mm,5μm);流动相:乙腈-水(64∶36);流速:1.0mL·min-1;检测波长:210nm。　在5.08～90.19μg·mL-1范围内峰面积与浓度呈良好的线性关系,稳定性良好,平均加样回收率为98.94%,RSD为2.95%;重复性RSD为1.49%。　该方法精密度高,分离度良好,可作为测定金边瑞香滴鼻剂中瑞香素含量的方法,为该制剂的质量控制提供了依据。[]　金边瑞香;瑞香素;高效液相色谱法;含量测定[]　R927.1;R286　　　[]　A　　　[]　1004-0781(2006)05-0457-03QualityStandardsofDaphneodoraThunbNoseDropsXIONGXue-min1,CAOJue2,ZHANGXiao-hui1,JIGang-feng3,ZHUJian-ping3,CHENLe1,SUNLei4(1.JiangxiProvincialInstituteofTraditionalChineseMedicineandMateriaMedica,Nanchang330077,China;2.JiangxiMedicalCollege,Nanchang330006,China;3.Classof2004SessionsforMastersGraduated,·457·20065255