UPLC法测定水红花子中花旗松素及槲皮素的含量

目的 应用超高效液相色谱法(UPLC)建立同时测定水红花子药材中花旗松素和槲皮素含量的方法。方法 采用Agilent ZORBAX SB-C18色谱柱,以乙腈-0.1%磷酸水为流动相梯度洗脱,柱温25℃,检测波长290 nm,流速0.2 mL·min^(-1),进样量1μL。结果 建立的分析方法方法学考察良好。花旗松素、槲皮素进样浓度分别在3.258~104.272μg·mL^(-1)、2.983~95.452μg·mL^(-1)内呈良好的线性关系(r~2=0.999 9),平均加样回收率为98.8%、98.8%,RSD值为1.9%、2.2%。结论 本方法简便、快速,可在同一波长下快速测定水红花子中花旗松素及槲皮素的含量,为水红花子药材质量控制提供参考依据。

Rapid Analysis of Four Alkaloids in Uncaria rhynchophylla by Core-Shell Column HPLC and Quantitative Analysis of Multi-Components by Single Marker(QAMS)

As a traditional herbal medicine,the major alkaloids in Uncaria rhynchophylla have been proven to have blood pressure-lowering and sedative effects.It is essential to develop an effective method for the determination of the major alkaloids in U.rhynchophylla.In this research,a rapid quantitative analysis involving multi-components analysis by a single marker strategy coupled with core-shell column HPLC was adopted to analyse four alkaloids(corynoxeine,isocorynoxeine,isorhynchophylline,rhynchophylline)in U.rhynchophylla.Isorhynchophylline was selected as the internal reference substance,the content of which was determined by the traditional external standard method.Relative correction factors(RCF)between isorhynchophylline and the other three alkaloids were calculated respectively.The results showed that the QAMS method had good robustness under different HPLC instruments.Nineteen batches of U.rhynchophylla were tested.No significant difference was observed between the results by QAMS and EMS(Correlation coefficient>0.99,p>0.05).The QAMS method could be employed as a rapid,effective technique for the quality control of U.rhynchophylla.

A Rapid Determination of 30 Prohibited Pesticide Residues in Lycii Fructus by UPLC-MS/MS

Prohibited pesticide residues have become one of the main factors affecting the quality and safety of Lycii Fructus,However,rarely studies focus on the rapid determination of these residues.Here,a total of 30 kinds of prohibited pesticide residues were determined by ultra-performance liquid chromatography tandem triple quadrupole mass spectrometry(UPLC-MS/MS)in five different process ways.Pretreatment methods,chromatographic separation and detection conditions in mass spectrometry were all optimized accordingly.Among the five different pretreatment methods,the first and third solid phase extraction failed to provide high recoveries of sulfosulfuron compounds(both lower than 60%).Recovery of chlorphenamidine by the Quick Easy Cheap Effective Rugged and Safe multiresidue method(QuEChERS)was lower than 60%,which did not meet the requirements of trace determination.The concentrations of 30 prohibited pesticides residues treated by straightforward and solid phase extraction showed good linearity in their corresponding ranges,with correlation coefficients over 0.99.The average recoveries of straightforward ranged from 78.13%to 110.9%,while RSD ranged from 1.3%to 16.9%,albeit poor purification was observed.The recovery yield from solid phase extraction was between 67.75%and 103.08%with RSD value from 0.8%to 14.0%,which met the requirements of trace determination,this method has good precision and stability.These results could be employed to other Traditional Chinese Medicines(TCMs)in detecting prohibited pesticide residues.

基于核壳色谱技术的葛根快速液相分析

目的采用核壳色谱技术建立葛根药材的快速液相分析方法,对2020年版中国药典含量测定指标葛根素进行快速定量分析,对主要色谱峰进行定性分析。方法选择PoroShell 120 SB-C_(18)(50 mm×4.6 mm,2.7μm)色谱柱,以甲醇-水(25∶75)为流动相,检测波长250 nm,流速1.0 mL·min^(-1),进样量2μL,采集频率5 Hz建立含量测定方法。采用四级杆-静电场轨道阱高分辨质谱对主要色谱峰进行指认。结果建立了葛根中葛根素含量8 min快速分析方法,鉴定了其中8个主要色谱峰,均为黄酮类化合物。葛根素定量分析方法线性关系、精密度、重复性、耐用性、加样回收率、稳定性均良好。核壳柱与常规色谱柱间的葛根素含量测定结果无显著差异,相较之下核壳色谱技术具有高效、低压等优势。结论该方法简单、快捷、准确、重复性良好,符合中国药典要求,可明显提升葛根样品中葛根素含量检测效率。