一测多评法同时测定健脾丸中4种有效成分的含量

Simultaneous determination of four kinds of active chemical compounds in Jianpi Wan by QAMS method

目的建立以党参炔苷为内参物,同时测定健脾丸中白术内酯Ⅰ、白术内酯Ⅱ、白术内酯Ⅲ含量的一测多评法(QA-MS)。方法2020年1月至2020年7月,采用高效液相色谱法,使用Zorbax SB-C_(18)(250.0 mm×4.6 mm×5μm),流动相为乙腈-水(含0.1%冰醋酸),线性梯度洗脱,流速1.0 mL/min,各检测成分的检测波长分别为党参炔苷(270 nm)、白术内酯Ⅰ(220 nm)、白术内酯Ⅱ(220 nm)和白术内酯Ⅲ(270 nm),柱温35℃,进样量10μL。结果白术内酯Ⅰ、白术内酯Ⅱ和白术内酯Ⅲ的相对校正因子(RCF)分别为0.804、0.627和1.715,相对保留时间(RRT)分别为1.259、1.312和1.551。各待测成分在9.937~198.740 mg/L(党参炔苷)、1.527~30.540 mg/L(白术内酯Ⅰ)、1.015~20.300 mg/L(白术内酯Ⅱ)、1.791~35.820 mg/L(白术内酯Ⅲ)范围内线性关系良好(r>0.999),平均回收率分别为98.16%、97.52%、98.18%、98.13%,相对标准差(RSD)分别为1.25%、1.05%、1.23%、1.08%。利用建立的方法与外标法分别测定10批次健脾丸中四种成分的含量结果一致。结论建立的QAMS操作简便,稳定性、精密度与重复性均良好,可用于健脾丸中白术与党参两种处方的质量控制。

Objective To establish aQAMS method for simultaneous multi-components determination of atractylodes macrolideⅠ,atractylodes macrolideⅡand atractylodes macrolideⅢin Jianpi Wan with lobetyolinas as the internal reference.Methods This study was conducted from January 2020 to July 2020,and high performance liquid chromatography was used with a Zorbax SB-C_(18)(250.0 mm×4.6 mm×5μm)column,the mobile phase was acetonitrile-water(0.1%acetic acid solution)at a flow rate of 1.0 mL/min with linear gradient elution.The detection wavelength of four kinds of components were 270 nm(for detection of lobetyolin and atractylodes macrolideⅢ)and 220 nm(for detection of atractylodes macrolideⅠand atractylodes macrolideⅡ),the column temperature was 35℃and the injection volume was 10 L.Results The relative correction factors(RCFs)of atracylenolide I,atracylenolideⅡand atracylenolideⅢwere 0.804,0.627 and 1.715,respectively,and their relative retention time(RRTs)were 1.259,1.312 and 1.551,respectively.It was linear for lobetyolin,atracylenolideⅠ,atracylenolideⅡand atracylenolideⅢin the range of 9.937-198.740 mg/L,1.527-30.540 mg/L,1.015-20.300 mg/L,1.791-35.820 mg/L(r>0.999).The average recoveries of four active components were 98.16%,97.52%,98.18%and 98.13%,with relative standard deviation(RSDs)of 1.25%,1.05%,1.23%and 1.08%,respectively.The method established in this paper was consistent with the external standard method for the determination of four components in 10 batches of Jianpi Wan.Conclusions The QAMS method is simple,precise,stable and reproducible.It can be used for the quality control of the two prescriptions of Atractylodes and Codonopsis in Jianpi Wan.