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.
关键词
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 polyphyllaICP-MSHPLCInorganic elementsPolyphyllinCorrelation