RP-HPLC法同时测定痢必灵片中6种成分的含量
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篇名: RP-HPLC法同时测定痢必灵片中6种成分的含量
TITLE:
摘要: 目的:建立同时测定痢必灵片中苦参碱、氧化苦参碱、没食子酸、芍药苷、木香烃内酯和去氢木香内酯含量的方法。方法:采用反相高效液相色谱法。色谱柱为Agilent ZORBAX SB-C18,流动相为甲醇-0.1%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为210 nm(苦参碱、氧化苦参碱)、225 nm(没食子酸、芍药苷、木香烃内酯、去氢木香内酯),柱温为30 ℃,进样量为5 μL。结果:苦参碱、氧化苦参碱、没食子酸、芍药苷、木香烃内酯和去氢木香内酯检测质量浓度线性范围分别为0.053~5.28 mg/mL(r=0.999 8)、0.125~12.54 mg/mL(r=0.999 9)、0.013~1.33 mg/mL(r=0.999 8)、0.169~16.94 mg/mL(r=0.999 9)、0.048~4.77 mg/mL(r=0.999 8)、0.072~7.16 mg/mL(r=0.999 9);定量限分别为4.08×10-4、4.48×10-4、3.12×10-4、2.10×10-4、1.36×10-4、1.84×10-4 mg/mL,检测限分别为1.24×10-4、1.50×10-4、1.02×10-4、6.20×10-5、4.20×10-5、6.40×10-5 mg/mL;精密度、稳定性、重复性试验的RSD均小于2%(n=6);加样回收率分别为98.03%~101.43%(RSD=1.25%,n=6)、97.73%~102.26%(RSD=1.96%,n=6)、97.18%~101.41%(RSD=1.98%,n=6)、97.45%~102.11%(RSD=1.88%,n=6)、96.85%~101.07%(RSD=1.75%,n=6)、97.12%~102.64%(RSD=1.82%,n=6)。结论:该方法操作简便,稳定、快速,可用于同时测定痢必灵片中6种成分的含量。
ABSTRACT: OBJECTIVE: To establish a method for simultaneous determination of matrine, oxymatrine, gallic acid, peoniflorin, costunolide and dehydrocostus lactone in Libiling tablets. METHODS: RP-HPLC method was adopted. The determination was performed on Agilent ZORBAX SB-C18 column with mobile phase consisted of methanol-0.1% phosphoric acid (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelengths were 210 nm (matrine, oxymatrine) and 225 nm (gallic acid, peoniflorin, costunolide, dehydrocostus lactone). The column temperature was set at 30 ℃, and sample size was 5 μL. RESULTS: The linear ranges of matrine, oxymatrine, gallic acid, peoniflorin, costunolide, dehydrocostus lactone were 0.053-5.28 mg/mL(r=0.999 8), 0.125-12.54 mg/mL(r=0.999 9), 0.013-1.33 mg/mL(r=0.999 8), 0.169-16.94   mg/mL(r=0.999 9), 0.048-4.77 mg/mL(r=0.999 8), 0.072-7.16 mg/mL (r=0.999 9). The limits of quantitation were 4.08×10-4, 4.48×10-4, 3.12×10-4, 2.10×10-4, 1.36×10-4, 1.84×10-4 mg/mL, respectively. The limits of detection were 1.24×10-4, 1.50×10-4, 1.02×10-4, 6.20×10-5, 4.20×10-5, 6.40×10-5 mg/mL, respectively. RSDs of precision, stability and reproducibility tests were all lower than 2% (n=6). The recoveries were 98.03%-101.43% (RSD=1.25%, n=6), 97.73%-102.26% (RSD=1.96%, n=6), 97.18%-101.41% (RSD=1.98%,n=6), 97.45%-102.11% (RSD=1.88%,n=6), 96.85%-101.07% (RSD=1.75%, n=6), 97.12%-102.64% (RSD=1.82%,n=6), respectively. CONCLUSIONS: Established method is simple, stable and rapid, and can be used for simultaneous determination of 6 components in Libiling tablets.
期刊: 2019年第30卷第4期
作者: 徐阳,单柏宇,鲍慧玮
AUTHORS: XU Yang,SHAN Baiyu,BAO Huiwei
关键字: 痢必灵片;反相高效液相色谱法;苦参碱;氧化苦参碱;没食子酸;芍药苷;木香烃内酯;去氢木香内酯;含量测定
KEYWORDS: Libiling tablets; RP-HPLC; Matrine; Oxymatrine; Gallic acid; Peoniflorin; Costunolide; Dehydrocostus lactone; Content determination
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