ABSTRACT
OBJECTIVE To establish the grade s tandard for Panax quinquefoli um and to evaluate the quality of different grades of medicinal materials. METHODS Totally 24 batches of P. quinquefolium were used as test samples. Pearson correlation analysis method was used to analyze the correlation between qualitative analysis indicators （taproot length ，taproot diameter and weight of single root ）and internal component indicators （ethanol-soluble extract ，and the contents of ginsenoside Rg 1，ginsenoside Re ， ginsenoside Rb 1，ginsenoside Rc ，ginsenoside Rb 2，ginsenoside Rd ，pseudo-ginsenoside F 11）. Combined with chemometrics methods，the reference indexes for the classification of P. quinquefolium were selected ，and the classification standards were formulated. HPLC-ELSD fingerprints of 24 batches of P. quinquefolium were established and their similarity evaluation was also performed. The chromatographic peaks were identified by comparison with the reference substance ，and then the quality of different grades of P. quinquefolium was evaluated by cluster analysis. RESULTS After screening ，taproot diameter ，the weight of single root and the content of ginsenoside Rd were taken as the reference indexes for the classification of P. quinquefolium . According to above 3 indexes，P. quinquefolium were divided into 3 grades：special grade ，first grade and second grade. According to the center value of K-means clustering ，the total score of special-grade medicinal materials was more than 135.40，that of first-grade medicinal materials was 61.82-135.40，and that of second-grade medicinal materials was less than 61.82. In the HPLC-ELSD fingerprints of 24 batches of P. quinquefolium ，25 common peaks were confirmed ，and 7 characteristic peaks were identified. The similarity of the chromatograms of P. quinquefolium of special grade ，first grade and second grade with fingerprints ranged 0.980-0.989，0.962-0.968，0.940-0.949，respectively. The results of cluster analysis showed that different grades of P. quinquefolium could be identified significantly. CONCLUSIONS The grade standard and HPLC-ELSD fingerprints of P. quinquefolium are established，which can be applied for exclusive identification of P. quinquefolium ，and provide reference for its quality control and grade classification.
ABSTRACT
OBJECTIVE:To establish the HPLC fingerprint for Anemone raddeana. METHODS:HPLC was performed on the column of Phemomenex Gemini C18 with mobile phase of 0.1%phosphoric acid-acetonitrile(gradient elution)at a flow rate of 1 ml/min,the detection wavelength was 206 nm,the column temperature was 30℃,and the injection volume was 20μl. With the refer-ence of raddeanin A,13 batches of A. raddeana were analyzed,chromatographic fingerprint similarity evaluation system software was conducted for similarity analysis,and SPSS 13.0 was conducted for cluster analysis. RESULTS:There were 11 common peaks in the 13 batches of A. raddeana with similarity of higher than 0.90. According to the verification,the fingerprint and control fin-gerprint shows good consistency. The drugs in Huadian,Jiaohe, Tiangang,Shulan,Tonghua and Fusong of Jilin and Shangzhi of Heilongjiang were regarded as category 1,and in Harbin,Yabuli town and Yimianpo of Heilongjiang,Qingyuan of Liaoning,Ji-nan of Shandong were category 2. CONCLUSIONS:The established fingerprint can provide reference for the identification and quality evaluation of A. raddeana.
ABSTRACT
OBJECTIVE:To establish a method for the contents determination of phospholipid and γ-linolenic acid in Com-pound linolenic acid soft capsule. METHODS:HPLC was conducted to determine the content of soybean lecithin;the column was Agilent TC-C18 with mobile phase of methanol-water(84:16,V/V)at a flow rate of 1.0 ml/min,the detection wavelength was 219 nm,the column temperature was 30 ℃,and the injection volume was 10 μl.Gas chromatography was conducted to determine the content of γ-linolenic acid in the preparation;the column was DB WAX,injector temperature was 210 ℃ by temperature pro-grammed,carrier gas was helium at a flow rate of 1 ml/min by split injection(split ratio of 1:30),and the injection volume was 0.02μl. RESULTS:The linear range was 4.64-16.24μg/ml for phospholipid(r=0.999 6)and 0.093 44-0.327 04μg/ml forγ-linole-nic acid methy ester(r=0.999 6);RSDs of precision,stability and reproducibility tests were lower than 3%;recoveries were 97.44%-99.36%(RSD=0.93%,n=6) and 97.22%-99.07%(RSD=1.01%,n=6),respectively. CONCLUSIONS:The method is simple,stable with good separation,and can be use for the contents determination of phospholipid and γ-linolenic acid in Com-pound linolenic acid soft capsule.
ABSTRACT
OBJECTIVE:To establish a method for the content determination of rosin acid in Rheumatoid arthritis tablet. METH-ODS:HPLC was performed on the column of ZORBAX SB-C18 with mobile phase of acetonitrile-0.1% formic acid(82∶18,V/V) at flow rate of 1.0 ml/min ,detection wavelength was 241 nm ,column temperature was 30 ℃ and volume injection was 10 μl. MS/MS column was ZORBAX SB-C18 with mobile phase of acetonitrile-0.1% formic acid(80∶20,V/V)at flow rate of 0.2 ml/min;column temperature was 30 ℃;volume injection was 0.5 μl. Ionization mode was ESI+,atomization gas pressure was 25 psi,gas flow as 8.0 L/min,capillary voltage was 4 000 V,capillary outlet voltage was 120 V,precursor ion was 303 m/z,scan range was 50-500 m/z and the gas temperature was 350 ℃. RESULTS:The linear range of rosin acid was 2.5-100.0 μg/ml. RSDs of preci-sion,stability and reproducibility tests were lower than 2.0%,recoveries was 96.75%-98.11%(RSD=0.53%,n=6). CONCLU-SIONS:The method is simple,accurate and reproducible,and suitable for the content determination of rosin acid in Rheumatoid arthritis tablet.