A comparison of the volatile compounds in Rhizomes Curcumae （Ezhu） and Radix Curcumae （Yujin） was undertaken using gas chromatography mass spectrometi-y （GC-MS）. Ultrasonic extraction and GC-MS methods were developed for the simultaneous determination of five sesquiterpenes, namely, α-pinene, β-elemene, curcumol, germacrone and curdione, in Ezhu and Yunjin. Good linearity （r〉0.999） and high inter-day precision were observed over the investigated concentration ranges. The validated method was successfully used for the simultaneous determination of five sesquiterpenes in Ezhu and Yujin. The quantitative method can be effectively used to evaluate and monitor the quality of Chinese curcuma in clinical use.
A global quality control method based on high performance liquid chromatography(HPLC)coupled with diode array detection(DAD),single quadrupole mass spectrometry(MS)and time-of-flight mass spectrometry(TOFMS)was developed for simultaneous determination of seven major components(mangiferin,neomangiferin,timosaponin E1,timosaponin E,timosaponin BⅡ,timosaponin BⅢ,and timosaponin AⅢ)and identification of most components in extracts of Rhizoma Anemarrhenae(RA).HPLC analysis was performed on an Agilent SB-C18 column(4.6 mm×150 mm,5 μm)by gradient elution using acetonitrile and water-acetic acid(100∶0.05,v/v)as the mobile phase.Seven major components in RA were successfully separated.This quantitative method was fully validated in respect of the following performance criteria:linearity,precision,repeatability,stability,accuracy,limits of detection(LOD)and quantification(LOQ).A formula database of known compounds in RA was established,against which,most of the reported components in this herbal extract were identified effectively based on the extract masses acquired by TOFMS.This qualitative and quantitative method was successfully used to analyze the components in 10 batches of RA samples collected from different regions in China.This global quality control method,which consisted of HPLC-DAD-MS assay of seven major components and unambiguous identification of nineteen components,is suitable for routine quantification and comprehensive quality control of RA.
Ke-Ren Wang1,Hai Zhang2,Zhen-Yu Zhu1,Zi-Yang Lou2,Liang Zhao1,Yi-Feng Chai1 1.Department of Pharmaceutical Analysis,School of Pharmacy,Second Military Medical University,Shanghai 200433
An offline two-dimensional system combining a rat cardiac mascle cell membrane chromatography time-of-flight mass spectrometry （CMC-TOF/MS） with a high performance liquid chromatography time-of-flight mass spectrometry （HPLC-TOF/MS） was established for investigating the parent components and metabolites in rat urine samples after administration of the roots of Aconitum carmichaeli. On the basis of the analysis of the first dimension, retention components of the urine sample were collected into 30 fractions （one fraction per minute）. Then offline analysis of the second dimension was carried out. 34 compounds including 24 parent alkaloids and 10 potential metabolites were identified from the dosed rat urine, and then binding affinities of different compounds on cell membranes were compared and influences of some functional groups on activity were estimated with the semi-quantification and curve fitting method. As a result, binding affinities decreased along with the process of deacylation, debenzoylation and demethylation, which may be related to the alleviation of toxicity in the procedure of herb processing or metabolism. Moreover, some minor components in rat urine （Songorine, 14-benzoylneoline, Deoxyaconitine, etc. ） exerted relatively strong affinity on cell membranes are worth exploring. The results delivered by the system suggest that the CMC can be applied to in vivo study.
Yan CaoXiao- Fei ChenDi- Ya LuXin DongGuo-Qing ZhangYi- Feng Chai
