ABSTRACT
Evaporative light scattering detector(ELSD) and charged aerosol detector(CAD) methods were established in this study for the content determination of four kinds of sugars in Zhusheyong Yiqi Fumai(YQFM), and the factors affecting the accuracy of CAD methods were discussed. HPLC-ELSD chromatographic separation was performed on a Shodex Asahipak NH2 P-50 column with acetonitrile-water(75∶25)as the mobile phase, with a flow rate of 0.8 mL·min~(-1), drift tube temperature of 80 ℃. The analysis by HPLC-CAD was performed on the same column with acetonitrile-water as mobile phase for gradient elution, with a flow rate of 0.8 mL·min~(-1), a neb temperature of 45 ℃, and power function(PF) of 1.3. The samples of YQFM were detected by ELSD and CAD respectively. It was found that YQFM was composed of fructose, glucose, sucrose and maltose. The linear relationship of the two methods was good, and the recoveries, reproducibility and stability of these four kinds of sugars measured by the two methods satisfied the requirements of methodology. Both CAD and ELSD detectors were accurate and reliable in detecting saccharides components in YQFM. In addition, it was revealed in this study for the first time that the PF parameter of CAD had an important influence on the accuracy of sugar determination and acted as the key parameter of CAD method. It was also found that for CAD, a non-linear detector, there was no significant difference between the results of linear regression and logarithmic regression.
Subject(s)
Aerosols , Carbohydrates , Chromatography, High Pressure Liquid , Light , Reproducibility of Results , Scattering, Radiation , SugarsABSTRACT
Objective::To establish the quality control method for multi-index content determination and fingerprint of salvianolic acids. Method::Agilent ZORBAX SB-C18 (4.6 mm×250 mm, 5μm) column was adopted, with 0.1%formic acid-water as mobile phase A and 0.1%formic acid-acetonitrile as mobile phase B for gradient elution (0-30 min, 20%-21.5%B; 30-35 min, 21.5%-25%B; 35-45 min, 25%-40%B; 45-50 min, 40%-95%B). The column temperature was set at 30 ℃, the flow rate was set at 1 mL·min-1, and the detection wavelength was set at 288 nm. Relative correction factors of caffeic acid, salvianolic acid E, rosmarinic acid, lithosperic acid, salvianolic acid B and salvianolic acid Y were determined by the concentration method. The content of each indicator component of the reference extract of salvianolic acid polyphenolic acid was determined and compared with the results of the monomer reference substance by the external standard method. At the same time, the fingerprint method was established. and the similarity evaluation was carried out on 10 batches of extracts. Result::Caffeic acid, salvianolic acid E, rosmarinic acid, lithospermic acid, salvianolic acid B, and salvianolic acid Y had a good linear relationship within the respective detection mass concentration ranges (r>0.999 9). The injection precision RSD was 0.1%-1.2%, the reproducible RSD was 1.2%-1.6%, and the recovery of the six components was 82.03%-98.68%. The stability of each component in the sample solution was good within 36 h. The relative correction factors for each indicator component were determined to be caffeic acid (2.92), salvianolic acid E (1.10), rosmarinic acid (1.61), lithosperic acid (1.07), salvianolic acid B (1.00), salvianolic acid Y (0.83). The effects of different methods, concentrations, instruments, columns, wavelengths were investigated, and the measured relative correction factors were found to be suitable. The results of the calibration factor method and the monomer standard reference substance method were less different. The HPLC fingerprints of the reference extract of salvianolic acids were established, and five common characteristic peaks were determined. The chromatographic peaks were confirmed according to the reference substance. The similarity of the fingerprints of the 10 batches of extracts was higher, and the quality difference was smaller. Conclusion::The multi-index content determination method and the fingerprint method established in this study are simple, rapid, accurate and reproducible, and can be used for quality control of Salviae miltiorrhizae Radix et Rhizoma polyphenolic acid reference extract.
ABSTRACT
The purpose of this study was to investigate the feasibility of the salvianolic acids reference extract for quality control for Salvia miltiorrhiza and salvianolic acids for injection. An Agilent ZORBAX SB-C18( 4. 6 mm×250 mm,5 μm) column was used with mobile phase consisting of 0. 1% formic acid-water and 0. 1% formic acid-acetonitrile in gradient elution procedure. The column temperature was 30 ℃; the flow rate was 1 m L·min-1; and the detection wavelength was 288 nm. The content of rosmarinic acid,lithospermic acid and salvianolic acid B in S. miltiorrhiza was determined by using the salvianolic acids reference extract as control substance. The content of caffeic acid,salvianolic acid E,rosmarinic acid,lithospermic acid,salvianolic acid B,and salvianolic acid Y in the salvianolic acids for injection was also determined. The linear relationship between chemicals was good( r>0. 998 9),and the injection precision RSD was 0. 30%-0. 90%. The sexual RSD is between 1. 4% and 3. 0%,and the RSD of the reproducibility of the extract is between 2. 1% and 5. 2%. The recovery rate of the three components in S. miltiorrhiza was 96. 80%-99. 20%,and the recovery rate of the six components in salvianolic acids for injection was 88. 90%-107. 5%. The solution of S. miltiorrhiza and salvianolic acids for injection were stable within 48 h. A total of 8 batches of S. miltiorrhiza and injection were determined by the reference extract,and the difference was smaller than that measured by the monomer control. This study preliminarily verified that the salvianolic acids reference extract can be used as a substitute for the monomer control for the quality control of S. miltiorrhiza and salvianolic acids for injection.
Subject(s)
Alkenes/analysis , Chromatography, High Pressure Liquid , Drugs, Chinese Herbal/standards , Polyphenols/analysis , Quality Control , Reproducibility of Results , Salvia miltiorrhiza/chemistryABSTRACT
To establish an on-line monitoring method for extraction process of Schisandrae Chinensis Fructus, the formula medicinal material of Yiqi Fumai lyophilized injection by combining near infrared spectroscopy with multi-variable data analysis technology. The multivariate statistical process control (MSPC) model was established based on 5 normal batches in production and 2 test batches were monitored by PC scores, DModX and Hotelling T2 control charts. The results showed that MSPC model had a good monitoring ability for the extraction process. The application of the MSPC model to actual production process could effectively achieve on-line monitoring for extraction process of Schisandrae Chinensis Fructus, and can reflect the change of material properties in the production process in real time. This established process monitoring method could provide reference for the application of process analysis technology in the process quality control of traditional Chinese medicine injections.
ABSTRACT
To study and establish a monitoring method for macroporous resin column chromatography process of salvianolic acids by using near infrared spectroscopy (NIR) as a process analytical technology (PAT).The multivariate statistical process control (MSPC) model was developed based on 7 normal operation batches, and 2 test batches (including one normal operation batch and one abnormal operation batch) were used to verify the monitoring performance of this model. The results showed that MSPC model had a good monitoring ability for the column chromatography process. Meanwhile, NIR quantitative calibration model was established for three key quality indexes (rosmarinic acid, lithospermic acid and salvianolic acid B) by using partial least squares (PLS) algorithm. The verification results demonstrated that this model had satisfactory prediction performance. The combined application of the above two models could effectively achieve real-time monitoring for macroporous resin column chromatography process of salvianolic acids, and can be used to conduct on-line analysis of key quality indexes. This established process monitoring method could provide reference for the development of process analytical technology for traditional Chinese medicines manufacturing.
ABSTRACT
Currently, near infrared spectroscopy (NIRS) has been considered as an efficient tool for achieving process analytical technology(PAT) in the manufacture of traditional Chinese medicine (TCM) products. In this article, the NIRS based process analytical system for the production of salvianolic acid for injection was introduced. The design of the process analytical system was described in detail, including the selection of monitored processes and testing mode, and potential risks that should be avoided. Moreover, the development of relative technologies was also presented, which contained the establishment of the monitoring methods for the elution of polyamide resin and macroporous resin chromatography processes, as well as the rapid analysis method for finished products. Based on author's experience of research and work, several issues in the application of NIRS to the process monitoring and control in TCM production were then raised, and some potential solutions were also discussed. The issues include building the technical team for process analytical system, the design of the process analytical system in the manufacture of TCM products, standardization of the NIRS-based analytical methods, and improving the management of process analytical system. Finally, the prospect for the application of NIRS in the TCM industry was put forward.