High Performance Liquid Chromatography gallbladder Capsule contents of baicalin
Author: Zhao Cuiyun Jia Yuan Li Chao Liu Yan Xin India
【Abstract】 Objective To study the choleretic Capsule baicalin method for the determination to develop quantitative quality control standards. Methods HPLC method for the preparation of the main drugs determination. Results The methodology of the system inspection and assay of three batches of samples to establish the product in the
determination of baicalin method, the measured three batches of samples of the contents of baicalin were 9.18,9.71,9.40 mg / tablets, baicalin its linear range of 19.7 ~ 98.5 μg / ml,
the regression equation: Y = 61 824X 75 898, r = 0.999. The average recovery was 100.3%, RSD 1.90%. Conclusion The established method has a specific, repeatable, no significant interference, etc., is to determine the gallbladder Capsule baicalin content in a more ideal way.
Key words gallbladder capsule; high-performance liquid
Determination of Baicalin in Lidan Capsule by HPLC
Abstract: ObjectiveTo study the method for determination of baicalin in Lidan Capsule and establish the pharmaceutical quality standard.MethodsThe main component of the pharmacy is
detected by HPLC.ResultsThe contents of baicalin in three batches of sample were 9.18 mg / capsule, 9.17 mg / capsule and 9.40 mg / capsule, respectively.The regression equation was Y = 61824X 75898, r = 0.999.The average recovery was
100.3%, RSD was 1.90%. ConclusionThe method is specific,
reproducible and noninterfered.It is a better method for determination of baicalin in Lidan Capsule.
Key words: Lidan Capsule; HPLC; Baicalin
Gallbladder capsule is being developed by the new Chinese
medicine, this product mainly by baicalin, cholic acid, HDCA and many other Chinese herbal medicines form. Jun Scutellaria-
based Prescription drugs, which contain baicalin is the main active ingredient , for the development of a quantitative
quality control standards of this drug with reference to relevant literature [2 ~ 5] in the determination of baicalin method, baicalin Lidan Capsule Assay carried out the study, through the methodology of systematic survey and assay of three batches of samples to establish the product of baicalin by HPLC method.
An instrument and reagent
United States Waters 600 high-performance liquid
chromatography (600 Pump, 996 Photodiode Array Detector); column of Shimadzu shim-pack CLC-ODS, 6.0 mm × 150 mm; ultra-
pure water; chromatography of pure methanol, and other reagents were analytically pure; baicalin reference substances were purchased in China's pharmaceutical and biological products.
2 Methods and Results
2.1 Preparation of sample solution
2.1.1 Preparation for the test product solutions appropriate to take this product, and research fine, saying that taking 0.2 g, precision that set, plus 70% ethanol, 40 ml, reflux extraction 3 h, put cold filtration, the filtrate
100 ml Liangping home in 70% ethanol with a small amount of sub-sub-washed containers and residues, filter into the same Liangping lotion, add 70% ethanol to scale, shake, as a solution for the test items.
2.1.2 Preparation of reference substance solution to take
60 ? vacuum drying 4 h the amount of baicalin reference substance buy 100 ml Liang Ping, the precision that as 19.70 mg, plus alcohol allows the dissolved and diluted to the scale, shake, as a reference substance stock solution; precise
volume of 3 ml set to take 10 ml Liang Ping, add methanol to the scale, shake, as a reference substance solution, its concentration of 59.10 μg / ml.
2.1.3 lack of preparation of Scutellaria blank solution and accurately according to the proportion of prescriptions
taken except that skullcap herbs outside the 3-pin to simulate
the preparation of this product technology and product solutions for the test preparation methods, made of skullcap missing blank solution.
2.2 Chromatographic conditions and system suitability
experiment octadecyl silane bonded silica gel as a filler; methanol -0.4% phosphoric acid solution (55:45) as mobile phase; flow rate of 1.0 ml / min; column temperature of 30 ? ; detection wavelength 280 nm. Number of theoretical
plates according to the calculation of baicalin peak should not be less than 2 000.
2.3.1 The maximum absorption wavelength of the alternatives are sophisticated drawing reference substance solution and test products for the solution of 10 μl, into
the sample, in the range of 200 ~ 370 nm to detect, depicts absorption diagram. The results showed that both at 280 nm at the maximum absorption peak detection wavelength was therefore determined to be 280 nm, and the "Chinese Pharmacopoeia" in
2005 edition of Part ? HPLC determination of baicalin in the same wavelength.
2.3.2 interference experiment, precision drawing a blank reference substance solution and test products for the solution and blank solution lacking the 10 μl, injection, and
detected at 280 nm, results show that the reference substance solution and test products for the solution at the wavelength are maximum absorption, while the lack of Scutellaria blank solution at the wavelength were no obvious peaks appeared,
indicating that under the conditions of the HPLC
determination, the determination of baicalin was no significant interference. Figure 1 ~ 3. Reposted elsewhere in the paper for free download http://
Figure 1 baicalin chromatography (abbreviated)
2.3.3 Precision linear relationship and the standard curve the amount of reserves to take the above-mentioned
reference substance solution 1,2,3,4,5 ml in 10 ml Liang Ping, add methanol to the scale, shake, their concentrations were 19.7,39.4, 59.1,78.8,98.5 μg / ml, more precise drawing
samples of each 10 μl, injection of high-performance liquid
chromatography, the measured peak area values. To peak area value of the vertical axis, sample volume (μg / ml) as
abscissa, drawing the standard curve regression equation was:
Y = 61 824X 75 898, r = 0.999, sample volume of 19.7 ~ 98.5 μ
g / ml the scope of a good linear relationship. The results in Table 1.
Figure 2 for the test materials chromatography (abbreviated)
Figure 3 missing skullcap blank chromatography
2.3.4 Precision Precision drawing experiment were tested with the product solution and the reference substance solution of 10 μl, respectively, continuous nebulization five times the value of measured peak area. The results for the test
items measured five times ? s = 3 288 247 ? 13 837.39, RSD
0.42%, reference substance measured five times ? s = 308 888
? 20 200.83, RSD 0.66%.
2.4 The stability of the experimental precision for the test items were drawn with the solution and reference
substance solution of 10 μl, at intervals of 2 h were
measured a second sample were measured five times, the peak area values in the determination of time, basically unchanged, within 8 h for the determination of test items five times ? s
= 3 317 748 ? 26 737.84, RSD 0.81%, reference substance measured five times ? s = 3 038 888 ? 20 200.83, RSD 0.66%,
indicating good stability.
Table 1 reference substance measured results (omitted)
2.5 repeated experiment to take the same group (20.05041
million) Sample 6 copies, according to determination under the law, samples were measured in the content of baicalin, the results of six determinations, the average content of 31.78 mg / g, the RSD was 2.4% , indicating good repeatability.
2.6 recovery experiment to take samples of five copies of the same batch, by adding 3.06 mg of baicalin (dubbed in the concentration of 1.02 mg / ml solution, accurate and adding 3.0 ml), according to the above method for the preparation of
the test items sample solution and determine the content of calculate the recovery rate. The results in Table 2.
Table 2 Addition recovery results (omitted)
2.7 Determination of the samples were drawn precision reference substance solution and three groups for the solution of the test product 10 μl, into the liquid chromatograph to
measure and calculate the various batches of samples the content of baicalin. The results in Table 3.
Table 33 groups gallbladder Capsule Determination of
baicalin in results (omitted)
Methodology of the system through the investigation and determination of samples was established in the preparation of baicalin HPLC assay method, measured by three batches of samples of the contents of baicalin were 9.18,9.71,9.40 mg / tablets, sample collection rate was 100.3%, the largest coefficient of variation was 1.90%.
The standard established by baicalin HPLC method for the determination, with specific, reproducible, no significant
interference, etc., is to control the inherent quality of this product an ideal way.
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