[生物医药论文精品]高效液相色谱法测定止痢宁片中脱水穿心莲内酯的含量

高效液相色谱法测定止痢宁片中脱水穿心莲内酯的含量摘要目的建立测定止痢宁片中脱水穿心莲内酯的高效液相色谱法。方法色谱柱DIAMONSILC18250NM46NM,5M甲醇水（6040）为流动相，流速为10MLMIN1，检测波长为254NM。结果在1029147GML1范围内线性关系良好（R099995，N7），平均回收率为9986，RSD199N6。结论该方法简便、准确、重现性好、精密度高，可用于止痢宁片中脱水穿心莲内酯的含量测定。关键词止痢宁片；脱水穿心莲内酯；高效液相色谱法含量测定HPLCQUANTITUTIVEDETERMINATIONFORZHILININGPIANABSTRACTOBJECTIVETOESTABLISHTHEHPLCQUANTITUTIVEDETERMINATIONFORTHEPAEONIFLORINCONTENTOFZHILININGPIANMETHODSCARRIEDOUTONADIAMONSILC18250NM46NM,5UMCOLUMNWITHMETHANOLWATER6040ASTHEMOBILPHASE,ANDDETECTIVEATTHEUVWAVELENGTHOF230NMRESULTSTHEMETHODOLOGICALSTUDYSHOWEDTHATAGOODLINERCORRELATIONFORTHEPAEONIFLORINEXISTEDINARANGEOF1029147UG/MLTHEAVERAGEOFPAEONIFLORINN6WAS9986ANDRSDWAS199CONCLUSIONTHEMETHODISSIMPLE,ACCURATEANDWITHGOODREPEATINGANDHIGHPRECISION,ANDCANBEUSEDFORTHEDETERMINATIONFORTHEPAEONIFLORINCONTENTOFZHILININGPIANKEYWORDSZHILININGPIAN14DEOXY11DEHYDROANDROGRAPHOLIDEHPLCCONTENTDETERMINATION止痢宁片收载于卫生部药品标准中药成方制剂第四册，具有清热祛湿，行气止痛的功效，用于肠炎、痢疾等。其处方中含有穿心莲、苦参、木香三味中药，现行质量标准中无含量测定项，为完善质量标准，控制产品的内在质量，确保临床疗效，本文建立了对止痢宁片中脱水穿心莲内酯的含量测定方法。1材料AGILENT1100SERIES高效液相色谱仪；METTLERAL104电子分G7524G3837G5191；SG37G22G2100G17241G3780清G8939G3132。脱水穿心莲内酯对G10043品G11013中G3281生G10301制品G7828定G6164G6564G1391G708G6221G25070G27G244G16G2100G2104，G1391含量测定用G709G11014G18267为色谱G13443水为G18337G14988G20323水，其G4439G16809剂G3355为分G7524G13443。止痢宁片3G6221G708G2338G3838药G1006有G19492G1856G2508，G6221G25070G260G22G22G25；四G5041G12178G18042G19463G1821制药有G19492G17143G1231G1856G2508，G6221G25070G260G2601；G8839G2347G5203G4443G2350G12197生G10301制药有G19492G1856G2508，G6221G25070G26010G21G709。2方法与结果21色谱G7477G1226色谱柱DIAMONSILC18250NM46NM,5M；G8981G2172相G11014G18267G713水G708G25040G709；G7828测G8886G19283254NM；柱G9213G21G24G263；G8981G1790710MLMIN1G17839G7691量10L。22脱水穿心莲内酯的含量测定参照中国药典2005年G10268G980G18108G256穿心莲片G257G20045G991收G17745的含量测定方法。221对G10043品G9354液的制G3803G12946G4506G12228G2474脱水穿心莲内酯对G10043品G17878量，G2164G11014G18267制成G86111ML含G1343475G的G9354液，G1328为对G10043品G9354液。222G1391G16809品G9354液的制G3803G2474本品20片G12946G4506G12228定，G11752G13466，G12946G4506G12228G2474G17878量G708G13434相G5415于G1016片的量G709，G13634具G3634G19193G5430G10954中，G12946G4506G2164G1849G11014G1826725ML，G4506G3634，G12228定G18337量，G9036G88851G4579G7114，G17241G3780处G10714G708功G10587250W，G20069G1058730KHZG70930分G19059，G6930G1931，G1889G12228定G18337量，用G11014G18267G15929G17287G1955G3845的G18337量，G6683G2260、G17819G9400、G2474G13505G9400液G2375G5483。223G19464G5627对G10043G9354液的制G3803G1209相G2528的处方G8616G1375制G5483G993含穿心莲的G12366G11345G7691品。G6365G1391G16809品G9354液的制G3803项G991的方法制成G19464G5627对G10043G9354液。224测定法分G2047G12946G4506G2572G2474G990G17860三G12193G9354液G252010L，G6365G990G17860色谱G7477G1226分G2047测定，见图1。结果表明G1391G16809品色谱图中呈现与脱水穿心莲内酯对G10043品保留G7114间相应的色谱峰，而G19464G5627对G10043无干扰。图A图B图C图1高效液相色谱图AG19464G5627对G10043；B对G10043品；CG1391G16809品FIG1HPLCCHROMATOGRAMSANEGATIVESAMPLEBSTANDARDCSAMPLE23线G5627关系考察G12946G4506G12228G2474脱水穿心莲内酯对G10043品147MG，G13634200ML棕色量G10954中，G2164G11014G18267G9354解并稀释至刻度，G6683G2260。G12946G4506G2572G2474G990G17860G9354液2，4，G25，G27，10，1G21，14LG17839G7691测定，记录峰面积。G1209浓度G708XG709对峰面积G708YG709G17839行线G5627回归，回归方程为Y1G249G21G22G21XG21G2614G22,R09999G24NG26，结果表明脱水穿心莲内酯对G10043品在1029147GML1范围内线G5627关系良好。24G12946G4506度G16809验G12946G4506G2572G2474对G10043品G9354液G252010L，连G13505G17839G76915次，G6164G5483峰面积值分G2047为11G250，11G249，11G251，11G250，11G250。结果峰面积G5191G3355值为11G250，RSD01NG24。25稳定G5627G16809验G12946G4506G2572G2474G990G17860G1391G16809品G9354液10L及对G10043品G9354液，于G214H后测定峰面积，结果峰面积几乎G993变，表明G1391G16809品G9354液至少在G214H内稳定。26G18337复G5627G16809验分G2047G12946G4506G12228G2474G2528一G7691品G708四G5041G12178G18042G19463G1821制药有G19492G17143G1231G1856G2508，G6221G2507G7080G260G2601G709G22份，G6365G1391G16809品制G3803项G991G17839行G6564G2474、制G3803、测定，测G5483含量G5191G3355值为036MG/片，RSD089N6。27G2164G7691回收G10587G16809验G12946G4506量G2474G2528一已知含量G7691品G708四G5041G12178G18042G19463G1821制药有G19492G17143G1231G1856G2508，G708G6221G25070G260G2601G709共G25份，分G2047G12946G4506G2164G1849G990G17860对G10043品G9354液G70807350MGML1）10ML，G10043G1391G16809品制G3803项G991G17839行G6564G2474、制G3803，并G6365G990G17860色谱G7477G1226测定，计算回收G10587，结果见表1。表1止痢宁片G2164G7691回收G10587G16809验结果TABG20RESULTSOFRECOVERYOFZHILININGPIANSAMPLEORIGINADDITIONGAINRECOVERYMEANRSD/MG/MG/MG/10587007350134811035420585107350131929986307354073501463799189986199407303073501448697825088540735016208100146088680735016120986428G7691品测定G6365G990G17860测定方法对3个厂家G7691品中脱水穿心莲内酯含量G17839行测定，结果见表2。表2止痢宁片中脱水穿心莲内酯含量测定结果TAB2DETERMINATIONRESULTSOFZHILININGPIANLOTCONTENT/MGRSD/0703361050590707010360890701020361513讨论31在G1391G16809品G9354液的制G3803方法选择G990，我们尝G16809了G6365本文方法制G3803后G2474G13505G9400液G2164在中G5627氧化铝柱G990，用G11014G18267G8939脱，收集G8939脱液，G2474G8939脱液G1889注G1849色谱仪测定，G6164G5483色谱图与本文方法G6164G5483色谱图相G8616较图G5430变化G993大，考虑到方法应方便易行选择了本文G1391G16809品G9354液的制G3803方法。32测定结果表明G993G2528的厂家脱水穿心莲内酯的含量相差较大，因此有必要建立脱水穿心莲内酯的含量测定，G1209G2164强药品质量的控制。参考文献1A1A0A3A4A2A5A3A7A6A8A11HPLCA12A9A10A15A13A