Glycerides are first separated to classes of triglycerides(TGs), diglycerides(DGs) and monoglycerides(MGs) by normal phase HPLC on silica gel column. Individual triglyceride separation is then achieved by non-aqueous ...Glycerides are first separated to classes of triglycerides(TGs), diglycerides(DGs) and monoglycerides(MGs) by normal phase HPLC on silica gel column. Individual triglyceride separation is then achieved by non-aqueous reversed phase(NARP) HPLC on C_(18) column with UV detection at 215nm.展开更多
目的建立复方制剂瑞格列奈二甲双胍片中二甲双胍有关物质的检查方法。方法采用HPLC法,色谱柱为CAPCELL PAK SCX(150 mm×4.6 mm,5.0μm);以0.35 mol·L-1磷酸二氢铵水溶液(用磷酸调节pH至3.0)为流动相进行等度洗脱,流速为1.0 m ...目的建立复方制剂瑞格列奈二甲双胍片中二甲双胍有关物质的检查方法。方法采用HPLC法,色谱柱为CAPCELL PAK SCX(150 mm×4.6 mm,5.0μm);以0.35 mol·L-1磷酸二氢铵水溶液(用磷酸调节pH至3.0)为流动相进行等度洗脱,流速为1.0 m L·min-1;采用紫外检测器,波长为210 nm。结果二甲双胍与有关物质A、B、C、D、E均能有效分离,分离度均大于1.5,且瑞格列奈不干扰有关物质的测定。结论该方法适用于该复方制剂中二甲双胍的有关物质控制。展开更多
High performance liquid chromatography was coupled with UV detection for simultaneous quantification of lopinavir （LPV） and ritonavir （RTV） in human plasma. This assay was sensitive, accurate and simple, and only ...High performance liquid chromatography was coupled with UV detection for simultaneous quantification of lopinavir （LPV） and ritonavir （RTV） in human plasma. This assay was sensitive, accurate and simple, and only used 200μL of plasma sample. Samples were liquid-liquid extracted, and diazepam was used as an internal standard. The chromatographic separation was achieved on a C18 reversed-phase analytic column with a mobile phase of acetonitrile-sodium dihydrogen phosphate buffer （10 mmol L-1, pH 4.80） （60：40, v/v）. UV detection was conducted at 205 nm and the column oven was set at 40℃. Calibration curves were constructed between 0,5-20 μg mL-1 for LPV and 0.05-5 μg mL-1 for RTV. The relative standard deviations were 2.16%-3.20% for LPV and 2.12%-2.60% for RTV for intra-day analysis, and 2.34%-4.04% for LPV and 0.31%-4.94% for RTV for inter-day analysis. The accuracy was within 100%＋10%. The mean extraction recoveries were 79.17%, 52.26% and 91.35% for RTV, LPV and diazepam, respectively. This method was successfully applied to human plasma samples from patients orally administered a salvage regimen of lopinavir-ritonavir tablets.展开更多
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
该实验采用LC-MS对银杏二萜内酯葡胺注射液原料中所含黄酮类成分的种类进行筛选,通过紫外-可见分光光度法（UV-Vis）和高效液相色谱法（HPLC-DAD）对银杏二萜内酯葡胺注射液原料中黄酮类成分限量检查灵敏度比较,发现HPLCDAD的检测限约为...该实验采用LC-MS对银杏二萜内酯葡胺注射液原料中所含黄酮类成分的种类进行筛选,通过紫外-可见分光光度法（UV-Vis）和高效液相色谱法（HPLC-DAD）对银杏二萜内酯葡胺注射液原料中黄酮类成分限量检查灵敏度比较,发现HPLCDAD的检测限约为UV-Vis的1/100,即HPLC-DAD检测灵敏度更高。基于LC-MS筛选结果选用槲皮素、山柰素和异鼠李素为对照品,采用Agilent Eclipse plus C18色谱柱（4.6 mm×250 mm,5μm）;0.4%磷酸-甲醇（50∶50）为流动相,等度洗脱;流速1.0 m L·min-1;检测波长360 nm。结果显示,此法专属性、精密度、重复性良好;槲皮素、山柰素和异鼠李素检测限分别为27.6,22.3,29.5μg·L-1;平均回收率在88.3%~91.7%;基于10批次样品检测结果和仪器灵敏度,最终确定银杏二萜内酯葡胺注射液原料中总黄酮醇苷的含量不得过2×10-5。该方法简便、快捷,可操作性好,可用于银杏二萜内酯葡胺注射液原料中黄酮类成分的限度检测。展开更多
文摘Glycerides are first separated to classes of triglycerides(TGs), diglycerides(DGs) and monoglycerides(MGs) by normal phase HPLC on silica gel column. Individual triglyceride separation is then achieved by non-aqueous reversed phase(NARP) HPLC on C_(18) column with UV detection at 215nm.
文摘目的建立复方制剂瑞格列奈二甲双胍片中二甲双胍有关物质的检查方法。方法采用HPLC法,色谱柱为CAPCELL PAK SCX(150 mm×4.6 mm,5.0μm);以0.35 mol·L-1磷酸二氢铵水溶液(用磷酸调节pH至3.0)为流动相进行等度洗脱,流速为1.0 m L·min-1;采用紫外检测器,波长为210 nm。结果二甲双胍与有关物质A、B、C、D、E均能有效分离,分离度均大于1.5,且瑞格列奈不干扰有关物质的测定。结论该方法适用于该复方制剂中二甲双胍的有关物质控制。
基金supported by the National Key Technologies R&D Program for the 11th Five-year Plan (Grant No. 2008ZX10001-006)the Key Clinical Program of the Ministry of Health 2010-2012
文摘High performance liquid chromatography was coupled with UV detection for simultaneous quantification of lopinavir （LPV） and ritonavir （RTV） in human plasma. This assay was sensitive, accurate and simple, and only used 200μL of plasma sample. Samples were liquid-liquid extracted, and diazepam was used as an internal standard. The chromatographic separation was achieved on a C18 reversed-phase analytic column with a mobile phase of acetonitrile-sodium dihydrogen phosphate buffer （10 mmol L-1, pH 4.80） （60：40, v/v）. UV detection was conducted at 205 nm and the column oven was set at 40℃. Calibration curves were constructed between 0,5-20 μg mL-1 for LPV and 0.05-5 μg mL-1 for RTV. The relative standard deviations were 2.16%-3.20% for LPV and 2.12%-2.60% for RTV for intra-day analysis, and 2.34%-4.04% for LPV and 0.31%-4.94% for RTV for inter-day analysis. The accuracy was within 100%＋10%. The mean extraction recoveries were 79.17%, 52.26% and 91.35% for RTV, LPV and diazepam, respectively. This method was successfully applied to human plasma samples from patients orally administered a salvage regimen of lopinavir-ritonavir tablets.
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。
文摘该实验采用LC-MS对银杏二萜内酯葡胺注射液原料中所含黄酮类成分的种类进行筛选,通过紫外-可见分光光度法（UV-Vis）和高效液相色谱法（HPLC-DAD）对银杏二萜内酯葡胺注射液原料中黄酮类成分限量检查灵敏度比较,发现HPLCDAD的检测限约为UV-Vis的1/100,即HPLC-DAD检测灵敏度更高。基于LC-MS筛选结果选用槲皮素、山柰素和异鼠李素为对照品,采用Agilent Eclipse plus C18色谱柱（4.6 mm×250 mm,5μm）;0.4%磷酸-甲醇（50∶50）为流动相,等度洗脱;流速1.0 m L·min-1;检测波长360 nm。结果显示,此法专属性、精密度、重复性良好;槲皮素、山柰素和异鼠李素检测限分别为27.6,22.3,29.5μg·L-1;平均回收率在88.3%~91.7%;基于10批次样品检测结果和仪器灵敏度,最终确定银杏二萜内酯葡胺注射液原料中总黄酮醇苷的含量不得过2×10-5。该方法简便、快捷,可操作性好,可用于银杏二萜内酯葡胺注射液原料中黄酮类成分的限度检测。
