RP-HPLC梯度洗脱法同时测定三七总皂苷及血塞通注射液中3种皂苷的含量

目的 :用高效液相色谱梯度洗脱法同时检测三七总皂苷原料及注射液中三七皂苷R1、人参皂苷Rb1、人参皂苷Rg13种皂苷含量 ,为重新修订质量标准中含量测定方法及含量限度提供了依据。方法 :用大连SpherisorbC8分析柱 ;乙腈 -水线性梯度洗脱 :0～ 3min (2 4∶76 ) ,3～ 15min (4 5∶5 5 ) ;流速 1 5mL·min-1;检测波长 2 0 3nm。结果 :该方法回收率三七皂苷R1为 99 8% ,人参皂苷Rb1为 10 0 6 % ,人参皂苷Rg1为98 9% ,RSD <1 1%。结论 :高效液相色谱梯度洗脱法能将多种皂苷很好地分离检测 ,提高了时效 ,减少了误差 ,结果表明该方法准确可靠 ,重现性好 ,结果稳定。

Simultaneous determination of ginsenosides Rg_1,Re and Rb_1 in rat plasma by HPLC and its application to pharmacokinetic study of SHENMAI injection

In the present study, we developed a sensitive and efficient high performance liquid chromatography （HPLC） method for the simultaneous determination of three ginsenosides （Rg1, Re, Rb1） in rat plasma. Chromatographic separation was performed on a C18 （150 min×4.6 mm） column utilizing gradient elution profile and a mobile phase consisting of （A） water and （B） acetonitrile. The calibration curve, with a great correlation coefficient greater than 0.998, was linear over the range of 1.0-30.0 μg/mL for ginsenoside Rgl, 0.5-15.0 μg/mL for ginsenoside Re, and 0.5-200.0 μg/mL for ginsenoside Rb1. The intra- and inter-day precisions for three ginsenosides （Rg1, Re, Rb1） were all less than 6.0%, and average recovery, examined at three concentration levels, ranged from 96.1% to 118.6%. The samples was stable within 24 h at 4 ℃ storage, and 30 d at -20 ℃ storage with three freeze-thaw-assay cycles. The low limits of quantification （LOQ） were 1.0, 0.5 and 0.5 μg/mL for Rg1, Re and Rb1, respectively. Taken together, the newly developed method was successfully applied to study the pharmacokinetics of ginsenoside Rg1, Re and Rb1 in rat plasma after intravenous administration of SHENMAI injection （SMI）.

参麦注射液中人参皂苷Rg_1和Re药代动力学研究

目的 研究参麦注射液中人参皂苷Rg1和Re人体药代动力学。方法 采用已建立的LC/MS/MS法同时测定人血浆中人参皂苷Rg1和Re浓度,并计算其药代动力学参数。结果 人参皂苷Rg1和Re线性范围为 1 023 -1 023μg·L-1和 1 05-1 050μg·L-1,方法回收率在 99% -105%和 99% -104%,日内、日间RSD值均小于 15%。参麦注射液 60mL经静脉滴注后人参皂苷Rg1和Re的药时曲线均符合二房室开放模型,T1 /2α分别为 0 28h和 0 10h,T1 /2β分别为 2 1h和 1 2h。结论 该法简便、灵敏、特异,适用于血浆中人参皂苷Rg1和Re浓度的测定。参麦注射液中人参皂苷Rg1和Re在人体内血药浓度较低,分布和消除速度较快,药代动力学行为符合二房室模型。

HPLC法测定中药血塞通氯化钠注射液中三种组分的含量

目的 建立血塞通氯化钠注射液的质量控制方法。方法 采用HPLC法测定制剂中的人参皂苷Rb1、人参皂苷Rg1和三七皂苷R1的含量。色谱柱为Shim -packCLC -ODS(4 .6× 2 5 0mm) ;测定人参皂苷Rb1流动相为 :乙腈 - 0 .0 5 %磷酸水溶液(35∶6 5 ) ;测定人参皂苷Rg1、三七皂苷R1流动相为 :乙腈 - 0 .0 5 %磷酸水溶液 (2 5∶75 ) ;流速为 1.5ml/min ;检测波长 2 0 3nm。结果 各组分峰面积与进样量呈良好线性关系。线性范围分别是 :人参皂苷Rb10 .79～ 3.94 μg ,人参皂苷Rg10 .6 2～ 3.2 1μg,三七皂苷R10 .6 5～ 3.5 7μg。平均回收率 :人参皂苷Rb110 0 .14 % ,RSD =0 .73% ;人参皂苷Rg199.6 6 % ,RSD =0 .72 % ;三七皂苷R110 0 .99% ,RSD =0 .5 9%。结论 本法简便、快速、灵敏、准确、重现性好 ,可作为该制剂的质量控制方法。