ABSTRACT
OBJECTIVE:To establish the HPLC fingerprint of Zhibai dihuang pills(concentrated pills),and to evaluate its quality. METHODS:The determination was performed on Dikma Diamonsil C18column with mobile phase consisted of 0.1%acetic acid solution-methanol(gradient elution)at the flow rate of 1.0 mL/min. The detection wavelength was set at 260 nm,and column temperature was 30 ℃. The sample size was 10 μL. Using paeonol as reference,HPLC chromatograms of samples from A, B,C manufacturers within validity period and samples from manufacturer A within validity period and out of validity period were drawn. The similarity of HPLC chromatogram for samples from A,B and C manufacturers and samples from A manufacturer within validity period and out of validity period was evaluated by TCM Chromatogram Fingerprint Similarity Evaluation System (2004 A). Common peaks of HPLC chromatogram for 3 manufacturers sample within validity period were confirmed. RESULTS:There were 24,29 and 32 common peaks in HPLC chromatograms for each 10 batches of samples from manufacturer A,B and C within validity period,respectively. The similarity of corresponding HPLC chromatograms of samples from manufacturer A,B and C compared with control HPLC chromatography were all higher than 0.94 with good agreement. HPLC chromatograms of sample from A manufacturer within validity period had good agreement with that from A manufacturer out of validity period. CONCLUSIONS:Established HPLC fingerprint analysis method can represent the quality of Zhibai dihuang pills (concentrated pills),but cannot effectively identify the expired samples.
ABSTRACT
This study was aimed to establish a rapid detection method for timosaponin BⅡ in Anemarrhenae Rhizoma in order to determine its concentration quickly,conveniently and efficiently.The concentration of timosaponin BⅡ in A.Rhizomadetected by HPLC in the Chinese Pharmacopeia was used as the actual measured value.The near-infrared spectroscopy (NIRS) was used to collect the spectrogram of A.Rhizomasamples.The partial least squares (PLS) of TQ Analyst 8.0 were used in the data analysis.Through the pretreatment,wavelength range and principal component number selection,the actual measured value and NIRS information were associated for the establishment of the optimal quantitative analysis model of timosaponin BⅡ.The results showed that the correlation coefficients (R2),root-mean-square error of calibration (RMSEC),root-mean-square error of prediction (RMSEP),root-mean-square error of cross-validation (RMSECV) and the performance index (PI) of the established model were 0.975 15,0.094 2,0.080 0,0.369 20,and 91.0,respectively.It was concluded that the established quantitative analysis model by NIRS with HPLC was able to determine the concentration of timosaponin BⅡ in A.Rhizomaquickly and accurately.
ABSTRACT
Objective To evaluate the performance of self‐established angiotensin converting enzyme (ACE) detection system . Methods The performance evaluation of ACE reagent kit produced by the Jiuqiang Company including precision ,linearity ,correla‐tion with the reference reagent and reportable range were conducted by using the automatic biochemical analyzer according to the re‐quirements of the EP5‐A2 and EP9‐A documentation in the Clinical and Laboratory Standards Institute (CLSI) .Results Intra‐as‐say CV of the system were 6 .87% ,2 .39% and inter‐assay CV were 6 .09% ,1 .81% ,respectively .During the day CV were 8 .00 %and 2 .8% respectively ,which were less than those provided by the manufacturer (<10% );the lenearity result was R2 =0 .99 .The correlation coefficient (r) of the system comparing with the reference reagent was 0 .990 56 ,moreover the average bias was 8 .55% , showing good correlation ;the repotable range was 9 .0U/L‐600U/L .Conclusion Self‐established ACE detection system can meet the requirements for clinical application .