摘要
目的:对LC-UV和LC-MS在山楂叶多元酚类成分分析中的应用进行方法学比较。方法:采用高效液相色谱并联双检测器(VWD和MSD)法。色谱柱为Lichrospher C18(250×4.6 mm I.D.,5μm);流动相A为乙腈,B为0.5%甲酸溶液,梯度洗脱,0-12 min A由11%-17%,12-30 min A由17%-18%,30-45 min A由18%-40%,45-60 minA由40%-100%;流速为1ml/min,三向分流阀分流进入MSD和VWD进行检测;柱温30℃;进样量10μl。结果:LC-MS灵敏度比HPLC法高10倍以上,在检测样品中微量成分时具有很大的优势;另外,LC-MS是根据tR和m/z两项指标来确定成分的类型,对于某些用LC-UV方法不能得到良好分离的组分或在LC-UV图谱上保留时间与对照品相近的其它成分,可以选用选择性离子检测(SIM)进行分析,能避免这些成分的干扰,因而具有高度的选择性和专属性。而LC-UV法操作简便,成本低,流动相选择面较广,因而分离度往往比LC-MS高,在检测样品中具有较好的紫外吸收、较好的分离度以及含量较高的成分时,LC-UV法以其高精密度和高稳定性完全可以达到LC-MS同样的检测结果。结论:LC-MS和LC-UV在山楂叶多元酚类成分的定量分析方面各有特色,可根据不同的检测指标选用不同的检测器。
Objective ： To compare the analytical method of LC-UV and LC-MS determination of major polyphenolic components in leaves of Crataegus L. Methods： By high-performance liquid chromatography method with VWD and MSD, Liehropsher C18 column （ 250 × 4. 6 mm I. D. , 5 μm） ; mobile phase consisted of solvent A （acetonitrile） and solvent B （0. 5 % formic acid） ; elution profile was： 0-12 min 11% to 17% A in B（linear gradient）, 12-30 min 17% to 18% A in B（linear gradient）, 30-45 min 18% to40% A in B（linear gradient）, 45-60 min 40% to 100% A in B（linear gradient） ; flow rate was 1.00 ml/min, flow into MSD and VWD by diffluence, column temperature 30℃ and the injection volume 10 μl. Result： The sensitivity of LC-MS was 10 times more than that of LC-UV, so it is preponderance for mieroanalysis. Additionally, because LC-MS can identify the component by retention time（tR ） and m/z, it has high selectivity and exclusion for the determined component. However, the method of LC-UV is simple; the cost is lower; the separate effect is better. So it is preponderance to determine the higher content component, which has better separate effect. Conclusion： LC-UV and LC-MS exhibited their own predominance for determination of major polyphenolie components in leaves of Crataegus L. So the detector should be selected according to the determined targets.
出处
《中药材》
CAS
CSCD
北大核心
2007年第3期285-289,共5页
Journal of Chinese Medicinal Materials
基金
国家自然科学基金资助项目(No.30472161)
江西省自然科学基金资助项目(No.0640163)
