超高效液相色谱-波长切换法同时测定健脾丸(浓缩丸)中4种成分的含量

Simultaneous Determination of Four Components in Jianpi Pills(Concentrated Pills)by UPLC-Wavelength Switching Method

目的建立同时测定健脾丸(浓缩丸)中党参炔苷、白术内酯I、白术内酯II、白术内酯III 4种成分含量的方法。方法采用超高效液相色谱法(UPLC),色谱柱为Poroshell 120 SB-C18(4.6 mm×100 mm,2.7μm),流动相为乙腈-0.1%乙酸,梯度洗脱,流速为0.5 ml/min,检测波长为270 nm(党参炔苷和白术内酯III)和220 nm(白术内酯I和白术内酯II),柱温为30℃,进样量为5μl。结果党参炔苷、白术内酯I、白术内酯II、白术内酯III检测线性范围分别为10.157~203.14μg/ml(r=0.9998),1.641~32.82μg/ml(r=0.9997),1.066~21.32μg/ml(r=0.9999),1.859~37.18μg/ml(r=0.9999),平均回收率分别为96.91%(RSD=1.71%,n=6),96.56%(RSD=1.39%,n=6),93.93%(RSD=1.71%,n=6),96.00%(RSD=1.66%,n=6),精密度、稳定性、重复性试验的RSD<2.0%。结论该方法重复性好、结果准确,可用于健脾丸(浓缩丸)的质量控制。

Objective To establish a UPLC method for simultaneous determination of lobetyolin,atracylenolide I,atracylenolide II and atracylenolide III in Jianpi Pills.Methods The chromatographic column was Poroshell 120 SBC18(4.6 mm×100 mm,2.7μm),using acetonitrile-0.1%acetic acid as the mobile phase of gradient elution.The flow rate was 0.5 ml/min.The detection wavelength was 270 nm(for determination of lobetyolin and atracylenolide III)and 220 nm(for determination of atracylenolide I and atracylenolide II),and the column temperature was 30℃.The injection volume was 5μl.Results The linear ranges for lobetyolin,atracylenolide I,atracylenolide II and atracylenolide III were 10.157-203.14μg/ml(r=0.9998),1.641-32.82μg/ml(r=0.9997),1.066-21.32μg/ml(r=0.9999),1.859-37.18μg/ml(r=0.9999),respectively.The average recoveries were 96.91%(RSD=1.71%,n=6),96.56%(RSD=1.39%,n=6),93.93%(RSD=1.71%,n=6),96.00%(RSD=1.66%,n=6),respectively.RSDs of precision,stability and reproducibility tests were lower than 2.0%.Conclusion The method is simple and accurate,can be used for simultaneous determination of four chemical components in Jianpi Pills.