中药化学成分定量分析方法学验证中精密度和准确度的探讨-王鹏

DrugStandardsofChina2010,Vol.11No.32010113191　　3　3.1　[2],4.36mg。28,144.36mg,50%,140.03～4.15mg,。3.2　[1],15mg。28,513.5mg,,17.9%;230.20～12.5mg/,82.1%,。3.3　HPLC,、,、、[3～6]。,、;、,、;,,,。3.4　2,。,,;、。,,。,,、。[1]　.《》2005.[S].328.[2]　.(2007002).[3]　,,,.RP-HPLC[J].,2005,27(9):1116-2.[4]　,,.HPLC、[J].,2001,23(6):445-448.[5]　,,,.[J].,2001,15(3):215-216.[6]　.HPLC[J].,2008,12(6):500-501.:,,。:。:13840195316。王鹏,宋宗华2,李清1,果德安3,钱忠直2,毕开顺1(1.,110016;2.,100061;3.,201203)　:研究精密度、准确度和范围的具体考察方法。:采用RP-HPLC法,以厚朴药材为例,对该药中厚朴酚、和厚朴酚含量进行测定,在方法学验证过程中,重复性和回收率试验分别设计不同范围和不同考察方法。:重复性试验结果表明厚朴酚、和厚朴酚含量的RSD分别为2.5%～5.8%,2.5%～5.7%;平均回收率厚朴酚为95.1%～97.7%(RSD=2.2%～4.3%);和厚朴酚为94.8%～97.7%(RSD=2.0%～7.5%)。:重复性RSD值随考察范围增大而增大,且同一浓度6份供试品溶液的测定结果与低、中、高浓度9份供试品溶液的测定结果方差非齐性。回收率RSD值亦随考察范围增大而增大。当药材取样量不同,根据被测成分含量按1:1添加对照品时,误差影响相对较小。而确定相同取样量,通过改变对照品加入量考察回收率时,9份样品测定结果RSD明显增大。:分析方法验证;精密度;准确度:921.2　　　:A　　　:1009-3656(2010)-3-191-5StudyonPrecisionandAccuracyinMethodValidationforQuantitativeAnalysisofCompo-nentsinTraditionalChineseMedicineWangPeng1,SongZong-hua2,LiQing1,GuoDe-an3,QianZhong-zhi2,BiKai-shun1(1.SchoolofPharmacy,ShenyangPharmaceuticalUniversity,Shenyang110016,China;2.ChinaPharmacopoeiaCommission,Beijing100061,China;3.ShanghaiInstituteofMateriaMed-2010113192　　DrugStandardsofChina2010,Vol.11No.3ica,ChineseAcademyofSciences,Shanghai201203,China)Abstract　Objective:Tostudythespecificinvestigationmethodofprecision,accuracyandrange.Methods:FordeterminationofthecontentsofmagnololandhonokiloincortexmagnoliaeofficinalisbyRP-HPLC,indifferentrange,therepeatabilityandaccuracywereevaluatedbydifferentmethods.Results:Formagnololandhonokilo,RSDsoftherepeatabilitywere2.5-5.8%and2.5-5.7%.Therangewithintentimes.Theaveragerecoverieswere95.1-97.7%,withRSDsof2.2-4.3%and94.8-97.7%,withRSDsof2.0-7.5%.Conclusions:RSDsoftherepeatabilityareincreasedastherangeenlarged,andthevarianceisnon-homogeneousbetween6and9determinedresults.RSDsoftherecoveriesareincreasedastherangeenlarged.Whentheratioofaddedandoriginalamountis1:1,theerrorislittlerelatively.Butifrecoveriesareinvestigatedbychangingaddedamountofreferencesubstance,RSDofthe9sampleresultsisobviouslyincreased.KeyWords:Analyticalmethodvalidation;Precision;Accuracy　　,,。《》2005[1],,,、,。,,,,。,[2]。,、,。1　Agilent1100,Agilent1100;SARTORIUSCP225D();YB-1A();SZ-93A()。(110729-200310)(110730-200609),;MagnoliaofficinalisRehd.etWils;();。2　:KromasilC18(4.6mm×200mm,5μm);:-(78∶22);:294nm;:1.0mL·min-1;:35℃;:5μL。,、1.5,,3800,1。3　3.1　对照品溶液的制备、,,1.125g·L-1、0.996g·L-1。、50mL,135.0mg·L-1、79.65mg·L-1。3.2　供试品溶液的制备()0.2g,,,25mL,,,24h,,5mL,25mL,,,。1　对照品(A)与供试品(B)的HPLC色谱图1.;2.4　4.1　线性关系考察0.5、1.0、2.0、4.0、8.0、10mL,10mL,,,,,,(C),DrugStandardsofChina2010,Vol.11No.32010113193　　(A),。:A=6.786C-1.764(r=1.000);:A=6.686C-1.008(r=1.000)。:、6.750～135.0mg·L-1、3.982～79.65mg·L-1。4.2　精密度试验4.2.1　　、、(6.750、27.00、108.0mg·L-1;3.982、15.93、63.72μg·mL-1),,6,RSD,0.8%、0.9%、0.8%;0.9%、0.7%、1.0%。4.2.2　　①6(n=6)。0.2g,,“3.2”6,,,、RSD,1。1　重复性试验结果(n=6)/%123456/%RSD/%　2.1842.2862.2352.2082.1712.1272.2022.51.2601.3071.2861.2751.2391.2201.2642.5　　②9(n=9)。10,“3.2”、、,3,,,、RSD,2。2　重复性试验结果(n=9)/%2.2592.2352.0101.2821.2841.148/%2.1681.238RSD/%5.85.74.3　加样回收率考察4.3.1　6(n=6)。0.1g,,6,2ml1.2mL,“3.2”,,,3。3　回收率试验结果(n=6)/mg/mg/mg/%/%RSD/%　2.2152.2504.34794.82.1952.2504.28893.02.2202.2504.30792.895.12.22.2042.2504.38697.02.2172.2504.35995.22.2062.2504.40997.91.2721.1952.4461.2601.1952.39995.31.2741.1952.41895.898.397.27.01.2651.1952.45099.21.2731.1952.43597.31.2671.1952.465100.32010113194　　DrugStandardsofChina2010,Vol.11No.34.3.2　9(n=9)。0.1g,,9,3,,“3.2”、、3,,,4。4　回收率试验结果(n=9)/mg/mg/mg/%/%RSD/%2.2021.1253.30497.6　2.2504.31493.595.62.73.3755.43495.61.2640.5971.83394.81.1952.42196.596.32.61.7923.01497.5　　0.03g、0.1g、0.3g,3,,9,,“3.2”、、3,,,5。5　回收率试验结果(n=9)/mg/mg/mg/%/%RSD/%0.6610.6751.33298.0　2.2022.2504.31493.596.73.06.6066.75013.2798.70.3790.3580.72394.31.2641.1952.42196.595.42.13.7923.5847.20895.3　　0.05g,,9,,,“3.2”、、3,,,6。6　回收率试验结果(n=9)/mg/mg/mg/%/%RSD/%1.1010.2251.31292.9　3.3754.42398.597.74.312.3813.68101.60.6320.1190.73685.71.7922.38397.894.87.56.5717.255100.84.4　稳定性试验,,DrugStandardsofChina2010,Vol.11No.32010113195　　0、2、4、6、8、12h,,、RSD0.8%、0.7%,12h。5　5.1　《》2005,,2.0%。[3,4],50%,10,。RSD,6、、9(P0.05)。,,。RSD。,1:1,。,,,,9RSD,,,RSD。,。,。5.2　,RSD,,。,。5.3　,,,。,,69RSD,9,,。[1]　.《》2005.[S].2005:ⅩⅧA.[2]　.[J].,2008,19(4):248.[3]　,.HPLC[J].,2007,21(5):338-339.[4]　,,,.[J].,2008,33(17):2087-2089.:,,,。[phone]。E-mail:[e-mail]。HPLC王国兰,寇晋萍,王俊秋,余立,周立春(,100035)　:建立反相高效液相色谱法测定复方氧氟沙星滴眼液中氧氟沙星和地塞米松磷酸钠的含量及有关物质。:反相高效液相色谱法,用资生堂SHISEIDOC18(UG120,4.6mm×250mm,5μm)色谱柱;以醋酸铵高氯酸钠溶液(取醋酸铵2.4g和高氯酸钠4.2g,用水900mL使溶解,用磷酸调pH值至2.5,再加水稀释至1000mL)-乙腈-甲醇(68∶22∶10)为流动相;检测波长有关物质为242nm和293nm,含量测定为254nm。:氧氟沙星和地塞米松磷酸钠的最低检测限分别为0.07ng和0.25ng;氧氟沙星在0.09～0.27g·L-1、地塞米松磷酸钠在0.03～0.09g·L-1的范围内浓度与峰面积呈良好的线性关系,线性回归方程分别为C=3.5×10-8A-4.5×10-3(r=1.000)和C=4.4×10-8A-1.1×10-4(r=1.000);两组分的回收率分别为100.1%和100.6%,相对标准偏差(RSD)为0.89%和1.32%。:本方法灵敏、准确、专属性强可用于测定复方氧氟沙星滴眼液中两组分的含量和有关物质。:氧氟沙星;地塞米松磷酸钠;反相高效液相色谱法:921.2　　　:A　　　:1009-3656(2010)-3-195-4