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目的基于一法多用策略,建立了在线二维多中心切割液相色谱同时测定三七、人参及其相关产品中人参皂苷Rg1、Re、Rf、Rb1、Rb2、Rb3、Rc、Rd的方法。方法按照产品的不同类别和制备工艺,分别采用相应的样品制备方法,对于原药材及其复方中药固体制剂,采用加压溶剂萃取法,分别采用三氯甲烷和水饱和正丁醇的2步溶剂提取;优化了一维和二维色谱分离条件,包括色谱柱选择、梯度洗脱等,分别采用Phenyl-x和C18柱作为一维和二维色谱柱,根据各目标物在一维色谱柱上的出峰时间,设置切割时间窗口,将各组分分别转移至6个定量环中,交替储存目标物馏分。第二维分离采用2.6μm颗粒的核-壳柱实现了8次的快速循环分离,完成8个目标物的测定。结果 8种目标待测物在药材、提取物和中药复方等基质均可获得较好的分离和定量,线性相关系数r>0.999,连续进样的精密度RSD在0.52%~1.53%,方法回收率在94.57%~103.47%,检出限在0.041~0.18μg/m L。结论本方法可准确对不同样品基质中的8种人参皂苷进行定量测定,结合8种人参皂苷的相对比例变化,可对人参、三七及其相关产品进行质量评价。
OBJECTIVE To establish a method for the simultaneous determination of ginsenosides Rg1, Re, Rf, Rb1, Rb2, Rb3, Rc and Rd in Panax notoginseng, ginseng and their related products by online two-dimensional polycentrifugation and liquid chromatography. Methods According to the different types of products and preparation process, the corresponding sample preparation methods were respectively adopted. For the crude drug and its compound traditional Chinese medicine solid preparation, pressurized solvent extraction method was used respectively, and the two-step solvent of trichloromethane and water saturated n-butanol Extraction and optimization of one-dimensional and two-dimensional chromatographic separation conditions, including column selection, gradient elution, respectively, Phenyl-x and C18 column as a one-dimensional and two-dimensional column, according to the target in a one-dimensional column Peak time, set the cutting time window, the components were transferred to six quantitative loop, alternate storage of the target fraction. The second dimension separation using 2.6μm particles of the core - shell to achieve a rapid eight cycles separation, the completion of the eight target determination. Results The eight target analytes were well separated and quantified in the matrix of herbs, extracts and traditional Chinese medicine compounds with the linear correlation coefficient r> 0.999 and the RSD of continuous injection between 0.52% and 1.53% The rates ranged from 94.57% to 103.47% with the detection limits of 0.041 ~ 0.18μg / m L. Conclusion This method can be used to quantitatively determine 8 kinds of ginsenosides in different sample matrices and to evaluate the quality of ginseng, notoginseng and their related products in combination with the relative proportion change of 8 kinds of ginsenosides.