Search Results
You are looking at 1 - 3 of 3 items for :
- Author or Editor: S. Li x
- Chemistry and Chemical Engineering x
- Refine by Access: Content accessible to me x
Summary
An efficient method used to separate five bioactive compounds from Gelidium amansii was optimized by the HCI software. The optimum composition of mobile phase for high-performance liquid chromatographic (HPLC) separation was obtained. The elution profiles were calculated by the polynomial theory based on the retention factor ln k = A + BF + CF 2 (F was the volume percentage of acetonitrile with 1.0% acetic acid); then, the theory was applied to calculate the elution profile in both isocratic and gradient modes by modifying different mobile phase conditions with HCI program. The calculated results of mobile phase condition suggested that acetonitrile-water (containing 1.0% acetic acid) with a linear gradient elution of 0∼30 min from 15:85 to 50:50 (v/v) was the optimized component. In the experimental conditions, the agreement between the experimental elution profiles and the calculated values of eluted concentration was relatively good.
A rapid and sensitive ultraperformance liquid chromatography-multiple reaction monitoring-multi-stage/mass spectrometry (UPLC-MRM-MS/MS) method has been developed for simultaneous quantification of salvianolic acid B and tanshinone IIA of salvia tropolone tablets in dog plasma. This was achieved by performing quantification using the MRM acquisition with two channels of MRM-MS/MS and MS full scan for more accuracy qualitative results, and the fragmentation transitions of m/z 295→249, 191 for tanshinone IIA and m/z 297→279, 251 for IS in positive mode, m/z 717→519, 321 for salvianolic acid B and m/z 295→267, 239 for IS in negative mode were selected. The UPLC separation was achieved within 3 min in a single UPLC run. Linear calibration curves were obtained over the concentration range of 10 pg/mL−1 ng/mL for tanshinone IIA and 100 pg/mL−1 for salvianolic acid B. Lower limit of quantitation (LLOQ) was 10 pg/mL and 100 pg/mL for tanshinone IIA and salvianolic acid B, respectively. The inter-day and intra-day precision (relative standard deviation, RSD) in all samples were less than 8.21%, and the recoveries were over 85.9% for both tanshinone IIA and salvianolic acid B. The two channels of MRM with MS full scan approach could provide both qualitative and quantitative results without the need for repetitive analyses and resulted in the reduction of further confirmation experiments and analytical time. The pharmacokinetic study of the two active components of salvia tropolone tablets following oral gavage administration of dogs was thus explored with this method.
An improved ion-pairing reversed-phase high-performance liquid chromatography method coupled with evaporative light scattering detection (HPLC-ELSD) was developed to determine spectinomycin and its related substances in commercial samples. The method was validated in accordance with International Conference on Harmonization (ICH) guidelines. The specificity of the HPLC-ELSD method was similar to that of the European Pharmacopoeia (Ph. Eur.) method, and repeatability and robustness were markedly improved relative to other reported methods due to our empirical evaluation of separation columns. Indeed, it is a more specific assay of spectinomycin than traditional microbiological techniques. The HPLC-ELSD method was used to evaluate the impurity profiles of eight compounds in seven spectinomycin batches from five different companies. Liquid chromatography coupled with electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) was employed to characterize the structures of these compounds. Though the HPLC-ELSD method was not as sensitive as the Ph. Eur. method, its limit of quantitation (LOQ) (0.16%) was lower than the disregard limit (0.3%) described by the Ph. Eur. 7.0. This suggests that the HPLC-ELSD method is appropriate for routine analysis of spectinomycin and its related substances.
