OBJECTIVE: To improve the quality standard for Qiwei maqianzi pills. METHODS: TLC was used for the qualitative identification of Chebulae Fructus and Aucklandiae Radix in the preparation. HPLC method was used for the content determination of hydroxy safflor yellow A, brucine and strychnine in preparation. The determination was performed on Phenomenex Prodigy C18 column with mobile phase consisted of methanol-acetonitrile-0.7% phosphoric acid soulution(26 ∶ 2 ∶ 72,V/V/V, for hydroxy safflor yellow A), acetonitrile-0.01 mol/L sodium heptanesulfonate mixed with same quantity of 0.02 mol/L potassium dihydrogen phosphate (pH adjusted to 2.8 using 10% phosphoric acid, 21 ∶ 79,V/V, for brucine and strychnine) at the flow rate of 1.0 mL/min. The detection wavelengths were 403 nm (for hydroxy safflor yellow A) and 260 nm (for brucine and strychnine). The column temperature was 25 ℃, and the injection volume was 10 μL. RESULTS: TLC spots of Chebulae Fructus and Aucklandiae Radix were clear and well-separated without interference from negative control. The linear range was 6.29-62.94 μg/mL for hydroxy safflor yellow A(r=0.999 3), 1.83-18.30 μg/mL for brucine(r=0.999 4) and 2.11-21.11 μg/mL for strychnine(r=0.999 6).RSDs of precision, stability and reproducibility tests were lower than 2.0%. The recoveries were 101.66%-104.91%(RSD=1.14%,n=6), 99.58%-104.55%(RSD=1.75%,n=6) and 101.22%-104.04%(RSD=0.99%,n=6), respectively. CONCLUSIONS: Improved standard can be better used for quality control of Qiwei maqianzi pills.
关键词
七味马钱子丸诃子木香羟基红花黄色素 A马钱子碱士的宁薄层色谱法高效液相色谱法质量标准
Keywords
Qiwei maqianzi pillsChebulae FructusAucklandiae RadixHydroxy safflor yellow ABrucineStrychnineTLCHPLCQuality standard