HPLC法同时测定六神丸中9种蟾蜍二烯内酯类成分的含量
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篇名: HPLC法同时测定六神丸中9种蟾蜍二烯内酯类成分的含量
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摘要: 目的:建立同时测定六神丸中和蟾蜍他灵、沙蟾毒精、远华蟾毒精、去乙酰华蟾毒它灵、蟾毒它灵、华蟾毒它灵、蟾毒灵、华蟾酥毒基、酯蟾毒配基含量的方法。方法:采用高效液相色谱法。 色谱柱为ODS-2 C18,流动相为乙腈-0.15%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为296 nm,柱温为40 ℃,进样量为10 μL。结果:和蟾蜍他灵、沙蟾毒精、远华蟾毒精、去乙酰华蟾毒它灵、蟾毒它灵、华蟾毒它灵、蟾毒灵、华蟾酥毒基、酯蟾毒配基检测质量浓度线性范围分别为1.10~70.39 μg/mL(r=0.999 6)、4.03~257.78 μg/mL(r=0.999 9)、4.09~261.89 μg/mL(r=0.999 9)、0.67~42.96 μg/mL(r=0.999 9)、3.36~214.73 μg/mL(r=0.999 9)、5.73~366.44 μg/mL(r=0.999 9)、3.77~241.56 μg/mL(r=0.999 9)、7.31~468.11 μg/mL(r=0.999 9)、5.18~331.56 μg/mL(r=0.999 9);定量限分别为1.10、0.85、1.02、0.34、0.84、1.43、0.94、3.66、2.59 μg/mL ,检测限分别为0.27、0.21、0.51、0.17、0.42、0.72、0.47、0.91、1.30 μg/mL;精密度、稳定性、重复性试验的RSD<3.0%;加样回收率分别为96.35%~103.10%(RSD=2.72%,n=6)、96.76%~103.24%(RSD=2.49%,n=6)、97.01%~101.39%(RSD=1.64%,n=6)、97.32%~104.01%(RSD=2.61%,n=6)、95.76%~103.60%(RSD=2.92%,n=6)、95.07%~102.59%(RSD=2.92%,n=6)、95.77%~101.43%(RSD=2.03%,n=6)、95.11%~103.72(RSD=3.19%,n=6)、95.23%~103.34(RSD=3.24%,n=6)。结论:该方法简便快速、准确可靠、重复性好,适用于同时测定六神丸中蟾蜍二烯内酯类成分的含量。
ABSTRACT: OBJECTIVE: To establish a method for simultaneous determination of gamabufotalin, arenobufagin, telocinobufagin, desacetylcinobufotalin, bufotalin, cinobufotalin, bufalin, cinobufagin and resibufogenin in Liushen pills. METHODS: HPLC method was adopted. The determination was performed on ODS-2 C18 column with mobile phase consisted of acetonitrile-0.15% phosphoric acid (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelength was set at 296 nm, and column temperature was 40 ℃. The sample size was 10 μL. RESULTS: The linear ranges of gamabufotalin, arenobufagin, telocinobufagin, desacetylcinobufotalin, bufotalin, cinobufotalin,bufalin, cinobufagin and resibufogenin were 1.10-70.39 μg/mL(r=0.999 6), 4.03-257.78 μg/mL(r=0.999 9),4.09-261.89 μg/mL(r=0.999 9),0.67-42.96 μg/mL(r=0.999 9),3.36-214.73 μg/mL(r=0.999 9), 5.73-366.44 μg/mL (r=0.999 9), 3.77-241.56 μg/mL (r=0.999 9),7.31-468.11 μg/mL (r=0.999 9),5.18-331.56 μg/mL(r=0.999 9). The limits of quantitation were 1.10, 0.85, 1.02, 0.34, 0.84, 1.43, 0.94, 3.66, 2.59 μg/mL; the limits of detection were 0.27, 0.21, 0.51, 0.17, 0.42, 0.72, 0.47, 0.91, 1.30 μg/mL, respectively. RSDs of precision, stability and reproducibility tests were all lower than 3.0%. The recoveries were 96.35%-103.10%(RSD=2.72%,n=6), 96.76%-103.24%(RSD=2.49%,n=6), 97.01%-101.39%(RSD=1.64%,n=6), 97.32%-104.01%(RSD=2.61%,n=6), 95.76%-103.60%(RSD=2.92%,n=6), 95.07%-102.59%(RSD=2.92%,n=6), 95.77%-101.43%(RSD=2.03%,n=6), 95.11%-103.72%(RSD=3.19%,n=6), 95.23%-103.34%(RSD=3.24%,n=6), respectively. CONCLUSIONS: The method is simple, rapid, accurate, reliable and can be used for the determination of bufadienolide in Liushen pills .
期刊: 2017年第28卷第21期
作者: 张宁,秦昆明,金俊杰,刘美辉,杨冰,曾庆琪
AUTHORS: ZHANG Ning,QIN Kunming,JIN Junjie,LIU Meihui,YANG Bing,ZENG Qingqi
关键字: 六神丸;蟾蜍二烯内酯类成分;含量测定;高效液相色谱法
KEYWORDS: Liushen pills; Bufadienolide; Content determination; HPLC
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