滇重楼药材中无机元素与有效成分的相关性研究
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篇名: 滇重楼药材中无机元素与有效成分的相关性研究
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摘要: 目的:研究滇重楼药材中无机元素与有效成分的相关性。方法:采用高效液相色谱法(HPLC)测定药材中重楼皂苷Ⅰ、Ⅱ、Ⅵ、Ⅶ的含量:色谱柱为Phenomenex C18,流动相为乙腈-水(梯度洗脱),流速为1.0 ml/min,检测波长为203 nm,柱温为30 ℃。采用电感耦合等离子体质谱法(ICP-MS)测定药材中钠(Na)、镁(Mg)、钾(K)、钙(Ca)、铬(Cr)、锰(Mn)、铁(Fe)、镍(Ni)、锌(Zn)、硒(Se)、锶(Sr)、钼(Mo)、铅(Pb)、镉(Cd)、汞(Hg)、铜(Cu)、砷(As)的含量:射频功率为1.55 kW,采样深度为10 mm,等离子气体流量为15.0 ml/min,载气流速为0.86 L/min,雾化室温度为2 ℃,碰撞模式为He,载气流量为4.5 ml/min,测量点数/峰为6,数据采样模式为跳峰采集(重复采集 3次)。所得数据采用SPSS 21.0软件进行逐步回归分析,以评价上述两者的相关性。结果:重楼皂苷Ⅰ、Ⅱ、Ⅵ、Ⅶ检测进样量线性范围分别为0.939~4.697 μg(r=0.999 9)、1.124~5.620 μg(r=0.999 6)、0.784~3.918 μg(r=0.999 8)、0.976~4.880 μg(r=0.999 9);精密度、稳定性、重复性试验的RSD<2%;加样回收率分别为96.53%~100.71%(RSD=1.69%,n=6)、98.19%~99.55%(RSD=0.58%,n=6)、95.45%~100.83%(RSD=1.87%,n=6)、96.11%~102.01%(RSD=2.07%,n=6)。17种无机元素检测含量线性范围为0~195.984 3 mg/kg(r≥0.999 3);检测限≤65.201 ng/kg。重楼皂苷Ⅰ含量与Mg呈正相关,与Pb呈负相关;重楼皂苷Ⅱ含量与Cu呈正相关,与As呈负相关;重楼皂苷Ⅵ含量与Sr、Hg呈正相关,与Mn呈负相关;重楼皂苷Ⅶ含量与Na、Ni呈正相关,与As呈负相关;4种重楼皂苷总含量与Ni、Sr呈正相关,与Fe呈负相关。结论:滇重楼药材中无机元素含量与有效成分存在一定相关性。
ABSTRACT: OBJECTIVE: To study the correlation of inorganic elements and active ingredients in Paris polyphylla. METHODS: HPLC was adopted for contents determination of polyphyllinⅠ, Ⅱ, Ⅵ and Ⅶ: the column was Phenomenex C18 with mobile phase of acetonitrile-water (gradient elution) at a flow rate of 1.0 ml/min, detection wavelength was 203 nm, and column temperature was 30 ℃. ICP-MS was adopted for contents determination of Na, Mg, K, Ca, Cr, Mn, Fe, Ni, Zn, Se, Sr, Mo, Pb, Cd, Hg, Cu and As: RF power was 1.55 kW, sampling depth was 10 mm, the plasma gas flow was 15.0 ml/min, carrier gas flow rate was 0.86 L/min, spray chamber temperature was 2 ℃, helium collision mode was He, gas flow was 4.5 ml/min, measurement points/peak was 6, sampling mode was hopping peak collection (repeated 3 times). And SPSS 21.0 software was adopted for stepwise regression analysis of correlation between the two above-mentioned. RESULTS: The linear range was 0.939-4.697 μg(r=0.999 8)for polyphyllinⅠ,1.124-5.620  μg(r=0.999 6) polyphyllinⅡ, 0.784-3.918 μg for polyphyllin Ⅵ,0.976-4.880 μg for polyphyllinⅦ.RSDs of precision, stability and reproducibility tests were lower than 2%, recoveries were 96.53%-100.71%(RSD=1.69%,n=6) for polyphyllinⅠ,98.19%-99.55%(RSD=0.58%,n=6) forⅡ, 95.45%-100.83%(RSD=1.87%,n=6) for polyphyllin  Ⅵ, 96.11%-102.01%(RSD=2.07%,n=6) for polyphyllin Ⅶ . The linear range was 0-195.984 3 mg/kg(r≥0.999 3),detection limit was no higher than 65.201 ng/kg. PolyphyllinⅠshowed positive correlation with Mg and negative correlation with Pb; polyphyllin Ⅱ showed positive correlation with Cu and negative correlation with As; polyphyllin Ⅵ showed positive correlation with Sr and Hg and negative correlation with Mn; polyphyllin Ⅶ showed positive correlation with Na and Ni and negative correlation with As; the total contents of the 4 polyphyllins showed positive correlation with Ni and Sr and negative correlation with Fe. CONCLUSIONS: The contents of inorganic elements and P. polyphylla have certain correlation with active ingredient.
期刊: 2016年第27卷第21期
作者: 沈昱翔,李果,李想,周浓,雷小宇
AUTHORS: SHEN Yuxiang1,LI Guo1,LI Xiang2,ZHOU Nong3,LEI Xiaoyu
关键字: 滇重楼;电感耦合等离子体质谱法;高效液相色谱法;无机元素;重楼皂苷;相关性
KEYWORDS: Paris polyphylla; ICP-MS; HPLC; Inorganic elements; Polyphyllin; Correlation
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