UPLC波长切换法同时测定小青龙颗粒中9种成分的含量

Simultaneous Determination of Nine Components in Xiaoqinglong Granules by UPLC with Wavelength Switching

目的:建立UPLC波长切换法同时测定小青龙颗粒中琥珀酸、盐酸麻黄碱、盐酸伪麻黄碱、芍药苷、甘草苷、甘草酸、桂皮醛、6-姜辣素和五味子醇甲的含量。方法:采用Agilent Zorbax C18色谱柱(100 mm×2.1 mm,1.8μm),以乙腈-0.1%磷酸溶液为流动相进行梯度洗脱,流速为0.5 ml·min-1,柱温为35℃。检测波长214 nm(0~8 min,琥珀酸、盐酸麻黄碱、盐酸伪麻黄碱),237 nm(8~15 min,芍药苷、甘草苷、甘草酸);285 nm(15~20 min,桂皮醛、6-姜辣素);250 nm(20~25 min,五味子醇甲)。结果:琥珀酸、盐酸麻黄碱、盐酸伪麻黄碱、芍药苷、甘草苷、甘草酸、桂皮醛、6-姜辣素和五味子醇甲的线性范围分别为1.37~54.72μg·ml-1(r=0.999 1)、2.58~103.20μg·ml-1(r=0.999 4)、1.71~68.48μg·ml-1(r=0.999 3)、5.81~232.32μg·ml-1(r=0.999 9)、3.25~129.92μg·ml-1(r=0.999 8)、2.35~93.92μg·ml-1(r=0.999 5)、1.18~47.07μg·ml-1(r=0.999 0)、1.98~79.04μg·ml-1(r=0.999 3)、2.28~91.36μg·ml-1(r=0.999 6);检测限分别为0.25,0.16,0.18,0.10,0.11,0.13,0.20,0.23,0.15μg·ml-1;定量限分别为0.40,0.20,0.21,0.14,0.15,0.18,0.35,0.38,0.19μg·ml-1;平均加样回收率分别为98.5%(RSD=0.9%)、101.1%(RSD=1.3%)、99.2%(RSD=1.7%)、101.7%(RSD=1.3%)、98.4%(RSD=0.5%)、98.2%(RSD=1.5%)、102.8%(RSD=1.4%)、97.0%(RSD=1.0%)、102.0%(RSD=0.8%)(n=9)。结论:本方法快速简便,精密度、稳定性及重复性好,实现了小青龙颗粒的多成分测定,为质量控制提供依据。

Objective:To establish a UPLC wavelength switching method for the simultaneous determination of succinic acid,ephedrine hydrochloride,pseudoephedrine hydrochloride,paeoniflorin,glycyrrhizin,glycyrrhizic acid,cinnamaldehyde,6-gingerol and schisandrin in Xiaoqinglong granules.Methods:The analysis was performed on an Agilent Zorbax C18 chromatographic column(100 mm×2.1 mm,1.8μm)with acetonitrile and 0.1%phosphoric acid as the mobile phase with gradient elution,the flow rate was 0.5 ml·min-1,and the column temperature was 35℃.The wavelength was 210 nm(0-8 min)for succinic acid,ephedrine hydrochloride and pseudoephedrine hydrochloride,237 nm(8-15 min)for paeoniflorin,lquiritin and glycyrrhizic acid,285 nm(15-20 min)for cinnamaldehyde and 6-gingero,and 250 nm(20-25 min)for schisandrin.Results:The linear concentration range of ephedrine hydrochloride,pseudoephedrine hydrochloride,paeoniflorin,liquiritin,glycyrrhizic acid,cinnamaldehyde,6-gingerol and schisandrin was 1.37-54.72μg·ml-1(r=0.999 1),2.58-103.20μg·ml-1(r=0.999 4),1.71-68.48μg·ml-1(r=0.999 3),5.81-232.32μg·ml-1(r=0.999 9),3.25-129.92μg·ml-1(r=0.999 8),2.35-93.92μg·ml-1(r=0.999 5),1.18-47.07μg·ml-1(r=0.999 0),1.98-79.04μg·ml-1(r=0.999 3)and 2.28-91.36μg·ml-1(r=0.999 6),respectively.The detection limit was 0.25,0.16,0.18,0.10,0.11,0.13,0.20,0.23,0.15μg·ml-1,the quantitative limit was 0.40,0.20,0.21,0.14,0.15,0.18,0.35,0.38,0.19μg·ml-1,and the average sample recovery was 98.5%(RSD=0.9%),101.1%(RSD=1.3%),99.2%(RSD=1.7%),101.7%(RSD=1.3%),98.4%(RSD=0.5%),98.2%(RSD=1.5%),102.8%(RSD=1.4%),97.0%(RSD=1.0%)and 102.0%(RSD=0.8%),respectively(n=9).Conclusion:The method is rapid,simple,accurate,stable and repeatable,and can be used to determine the components of Xiaoqinglong granules.