School of Pharmacy, East China University of Science and Technology, PR China.
J Pharm Biomed Anal. 2010 May 1;52(1):66-72. doi: 10.1016/j.jpba.2009.12.017. Epub 2009 Dec 29.
A new method using ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC/Q-TOF-MS) was developed for the rapid qualitative and quantitative analyses of Asian ginseng (Panax ginseng C.A.Meyer) in adulterated American ginseng (Panax quinquefolium L.) preparations within 2min. The method was based on the baseline chromatographic separation of isomeric compounds of ginsenoside Rf and 24(R)-pseudoginsenoside F(11), two potential chemical markers present in Panax ginseng C.A.Meyer and P. quinquefolium L. methanolic extracts. The chromatographic separation was achieved by UPLC, which used a column with 1.7microm particle packing which enabled the higher peak capacity, greater resolution, increased sensitivity and higher speed of analysis. Ginsenoside Rf and 24(R)-pseudoginsenoside F(11) were separated on baseline with retention times of 1.5 and 1.7min, respectively. Ginsenoside Rf and 24(R)-pseudoginsenoside F(11) were identified and conformed unambiguously by accurate mass measurement and their different fragmentation pathways were performed on Q-TOF-MS. Quantitative analysis was carried out under selective ion monitoring (SIM) mode. The limit of detection (LOD) of this UPLC/Q-TOF-MS analysis for ginsenoside Rf and 24(R)-pseudoginsenoside F(11) was 0.05 and 0.08ng, respectively. Ginsenoside Rf was linear over the range of 0.164-16.4ng with a correlation coefficient (R(2)) of 0.9997, while 24(R)-pseudoginsenoside F(11) was linear from 0.243 to 24.3ng with an R(2) of 0.9989. Furthermore, inter-day and intra-day precisions were obtained below 4.0% and the analytical method was fully validated. 12 batches of self-prepared adulterated samples, 11 batches of Asian ginseng, 16 batches of American ginseng and 13 batches of commercial American ginseng preparations were tested. The method developed is rapid, accurate, reliable and highly sensitive for qualitative and quantitative analyses of Asian ginseng and American ginseng.
一种使用超高效液相色谱四极杆飞行时间质谱(UPLC/Q-TOF-MS)的新方法已经被开发出来,用于在 2 分钟内快速定性和定量分析掺伪美国人参制剂中的亚洲人参(Panax ginseng C.A.Meyer)。该方法基于人参皂苷 Rf 和 24(R)-伪人参皂苷 F(11)的异构体化合物的基线色谱分离,这两种潜在的化学标志物存在于 Panax ginseng C.A.Meyer 和 P. quinquefolium L.的甲醇提取物中。色谱分离通过 UPLC 实现,该方法使用了 1.7μm 颗粒包装的柱,可提高峰容量、分辨率、灵敏度和分析速度。人参皂苷 Rf 和 24(R)-伪人参皂苷 F(11)分别在保留时间为 1.5 和 1.7min 时基线分离。通过准确质量测量和不同的碎片途径,对人参皂苷 Rf 和 24(R)-伪人参皂苷 F(11)进行了鉴定和明确确认。定量分析采用选择离子监测(SIM)模式进行。该 UPLC/Q-TOF-MS 分析对人参皂苷 Rf 和 24(R)-伪人参皂苷 F(11)的检测限(LOD)分别为 0.05 和 0.08ng。人参皂苷 Rf 在 0.164-16.4ng 范围内呈线性,相关系数(R²)为 0.9997,而 24(R)-伪人参皂苷 F(11)在 0.243-24.3ng 范围内呈线性,R²为 0.9989。此外,日内和日间精密度均低于 4.0%,分析方法得到了充分验证。测试了 12 批自制掺伪样品、11 批亚洲人参、16 批美国人参和 13 批商业美国人参制剂。该方法快速、准确、可靠,对亚洲人参和美国人参的定性和定量分析具有高度灵敏度。