[Quality evaluation of fried Glycyrrhizae Radix et Rhizoma pieces by HPLC fingerprint and multicomponent quantitative analysis].

To establish the HPLC fingerprint and multi-component determination method of fried Glycyrrhizae Radix et Rhizoma pieces. HPLC analysis was performed on Thermo Acclaim ~(TM)120 C_(18) column(4.6 mm×250 mm, 5 µm). Acetonitrile-0.1% phosphoric acid aqueous solution was taken as the mobile phase for gradient elution. The flow rate was 1 mL·min~(-1),the column temperature was maintained at 30 ℃, and the detection wavelength was 237 nm and 360 nm. The similarity of 15 batches of fried Glycyrrhizae Radix et Rhizoma pieces was higher than 0.849, and 17 common peaks were identified. Liquiritin, isoliquiritin apioside, isoliquiritin, liquiritigenin, isoliquiritigenin and glycyrrhizic acid were identified; among them, the mass fractions of Liquiritin, isoliquiritin apioside, isoliquiritin, liquiritigenin, glycyrrhizic acid were were 0.519%-3.058%, 0.227%-0.389%, 0.070%-0.439%, 0.038%-0.173%, 1.381%-4.252%, respectively. According to the cluster analysis, the 15 batches of decoction pieces were classified into three categories; principal component analysis screened out four principal components, with the cumulative variance contribution rate of 86.630%, indicating that the principal components contained most information of original data. Partial least squares discriminant ana-lysis marked 6 differential components in the decoction pieces. The established fingerprint and multicomponent determination are stable and reliable, and can provide a reference for the quality control of Radix Glycyrrhizae Radix et Rhizomae and fried Glycyrrhizae Radix et Rhizoma pieces.

[Tissue Distribution of Alkaloids from Coptidis Rhizoma in Rats Determined by UPLC-MS].

Objective: To develop an UPLC-MS method for simultaneous determination of alkaloids from Coptidis Rhizoma in rat tissues, and to study the tissue distribution of alkaloids from Coptidis Rhizoma in rats. Methods: The samples were extracted with ethyl acetate, and analyzed by UPLC-MS with acetonitrile-0. 2% formic acid solution in a gradient elution mobile phase, the flow rate was 0. 2m L/min. Tetrahydropalmatine was used as an internal standard. The mass spectrometer was operated in selected reaction monitoring( SIM) mode with positive electrospray ionization, the transition were m/z 191. 904 /118. 973( noroxyhydrastinine), m/z 335. 877 /308. 072( 8-ocoptisine),m/z 351. 94 /294. 554( palmatine chloride),m/z 335. 94 /262. 112( epiberberine), m/z 337. 94 /322. 422( columbamine), m/z 319. 904 /292. 037( coptisine), m/z 355. 977 /192. 036( tetrahydropalmatine),m/z 335. 94 /320. 036( berberine hydrochloride),m/z 351. 94 /321. 995( oxyberberin), m/z 337. 94 /322. 949( jatrorrhizine respectively). Results: Excellent linearity was observed in all alkaloids in their linear range( r & 0. 9901). The RSD of precision of the developed method was less than 15%,and the accuracy and stability were less than ± 15%,the extraction recovery was 72. 1% ~ 82. 9% with RSD less than 15%. Coptisine,epiberberine,berberine,jatrorrhizine,columbamine,palmatine were widely distributed in rat tissues. Noroxyhydrastinine,8-ocoptisine,oxyberberin could only be determined in liver and heart or kidney. Conclusion: The established method is simple and accurate. Satisfactory results are obtained with applying this method to the tissue distribution study of alkaloids from Coptidis Rhizoma.

[Common and variant peak ratios in IR fingerprint of Cacumen platycladi with dual-index sequence analysis].

To establish a new method to analyze IR fingerprint, which is in line with the characteristic of traditional Chinese medicine, two indexes, common peak ratio and variant peak ratio, were applied and their values were calculated by means of sequential analysis, in which each Cacumen platycladi sample's IR fingerprint spectra were set up and the common peak ratio sequences were arranged in the order of size in comparison with other samples. The analytical results showed that samples G1 and G8 from the same region, and G4, G2 and G6 from the closer regions were the most similar samples with higher common peak ratio (> or = 90.0%) and lower variant peak ratio (< or = 11.1%). However, the samples G10, G3, G4 and G5 from the closer regions collected in different years, and G2 and G7 from the farther regions,were of significant disparity with common peak ratio less than 50% and variant peak ratio larger than 50%. As a result, the method could be used to distinguish Cacumen platycladi of different areas and batches. The dual index sequential analysis enables us to distinguish two or more herb's IR fingerprints, is a new method to analyze IR fingerprint spectra, and can be used in line with the characteristics of traditional Chinese medicine.

[Determination of donepezil in human plasma by HPLC-MS].

AIM: To establish a sensitive and specific liquid chromatography-mass spectrometry (time-of-flight) [LC-MS (TOF)] method for the determination of donepezil in human plasma after an oral administration of 5 mg donepezil hydrochloride tablet. METHODS: Alkalized plasma was extracted with isopropanol-n-hexane (3:97) and loratadine was used as internal standard. Solutes were separated on a C18 column with a mobile phase of methanol-acetate buffer (pH 4.0) (80:20). Detection was performed on a time-of-flight mass spectrometry equipped with an ESI interface and operated in positive-ionization mode. Donepezil quantitation was realized by computing the peak area ratio (donepezil-loratadine) (donepezil m/z 380[M + H]+ and loratadine m/z 383[M + H]+) and comparing them with calibration curve (r = 0.9998). RESULTS: The linear calibration curve was obtained in the concentration range of 0.1-15 micrograms.L-1. The detection limit of donepezil was 0.1 microgram.L-1. The average recovery was more than 90%. The intra- and inter-run precision was measured to be below 15% of RSD. CONCLUSION: The method is sensitive, simple and rapid, so, it can meet the need of the studies on the pharmacokinetics and bioavailability of donepezil.