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1...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。展开更多
[Objectives] To determine the nine phenolic components in the leaves of Crataegus pinnatifida Bge. [Methods] The reversedphase high-performance liquid chromatography( RP-HPLC) was applied. [Results] Nine phenolic comp...[Objectives] To determine the nine phenolic components in the leaves of Crataegus pinnatifida Bge. [Methods] The reversedphase high-performance liquid chromatography( RP-HPLC) was applied. [Results] Nine phenolic components showed a good linear relationship in the range of 2-500 μg/m L with r in the range of 0. 999 5-0. 999 9. The recovery rate of spiked samples ranged from 93. 7% to110. 2%,and the relative standard deviation was in the range of 0. 69%-4. 58%. The leaves of 29 cultivars of C. pinnatifida Bge. were measured,and the average content of the nine phenolic components was as follows: isoquercitrin,hyperoside,procyanidin C1,procyanidin D1,epicatechin,procyanidin B2,chlorogenic acid,eucomic acid,and vitexin 2 "-O-rhamnoside. The contents of flavonoids and phenolic acids were high,up to 15 mg/g D. W,and the content of procyanidins was up to 6 mg/g D. W. [Conclusions]This method is easy and accurate in determination of phenolic components in the leaves of C. pinnatifida Bge.展开更多
文摘目的: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。
基金Supported by Project of Natural Science Foundation of Hebei Province(C2015204187)
文摘[Objectives] To determine the nine phenolic components in the leaves of Crataegus pinnatifida Bge. [Methods] The reversedphase high-performance liquid chromatography( RP-HPLC) was applied. [Results] Nine phenolic components showed a good linear relationship in the range of 2-500 μg/m L with r in the range of 0. 999 5-0. 999 9. The recovery rate of spiked samples ranged from 93. 7% to110. 2%,and the relative standard deviation was in the range of 0. 69%-4. 58%. The leaves of 29 cultivars of C. pinnatifida Bge. were measured,and the average content of the nine phenolic components was as follows: isoquercitrin,hyperoside,procyanidin C1,procyanidin D1,epicatechin,procyanidin B2,chlorogenic acid,eucomic acid,and vitexin 2 "-O-rhamnoside. The contents of flavonoids and phenolic acids were high,up to 15 mg/g D. W,and the content of procyanidins was up to 6 mg/g D. W. [Conclusions]This method is easy and accurate in determination of phenolic components in the leaves of C. pinnatifida Bge.
