High Performance Liquid Chromatography Qingrejiedu Oral baicalin content
【Abstract】 Objective To establish Qingrejiedu baicalin oral method for the determination. Methods The study methodology to establish Qingrejiedu HPLC Determination of baicalin content
in oral method. The results of baicalin in the range of 0.12 ~ 0.72 μg good linear relationship, the average recovery was 95.8%, RSD of 0.87% (n = 6). Conclusion The separation of effective, accurate and reliable.
Key words Qingrejiedu oral; baicalin; high-performance liquid
chromatography
Determination of Baicalin in Qingrejiedu Oral Solution by HPLC
Abstract: ObjectiveTo measure the content of Qingrejiedu Oral Solution by HPLC. MethodsHPLC was used.ResultsA good
linear relationship was obtained within the range of 0.12 ~ 0.72 μg, and the average recovery was 95. 8%, RSD = 0.87% (n = 5 ). ConclusionThe method can separate effectively, and the result is accurate and reliable.
Key words: Qingrejiedu Oral Solution; Baicalin; HPLC
Qingrejiedu oral solution [1], through clinical testing with a heat-clearing and detoxifying, YangYinShengJin and Cooling Sanjie such effect, consistent with the formation of a variety of hot card pathogenesis of a variety of fever showed
significant effects of the disease. The prescription from the gypsum, Anemarrhena, Huang Qin, gardenia, gentian, etc. 12
medicinal flavor composition, has been used in the clinical years, its curative effect [2].
Skullcap for Fong main drug used to clear diarrhea triple burner hot, the main active ingredient of baicalin, baicalin have chosen to target as a determination of the quality control of heat-clearing and detoxifying oral liquid. This paper intends to use HPLC determination Qingrejiedu oral
liquid content of baicalin.
1 Equipment
Shimadzu LC 10ATvp series of high-performance liquid
chromatography (Japan); N2000 high-performance liquid
chromatography workstation (USA); Satrous electronic balance (Switzerland); DL 360 Ultrasonic Cleaner (Ningbo City,
Shipu Haitian Electronic Instrument Factory) ; JP A-type
frame-pan balance scales (Taicang City, the East Asian Balance Instrument Co., Ltd.).
Qingrejiedu Oral Liquid (self); baicalin (Chinese medicines and biological products); methanol liquid chromatography with reagents, deionized water twice re-
distilled water, and other reagents were of analytical grade.
2 Methods and Results
2.1 Chromatographic conditions Column: IOSOHOC18 (150 mm × 4.6 mm, 5 μm) (Japan); mobile phase: methanol water-
phosphoric acid (50:50:0.3); detection wavelength: 276 nm; column temperature: 35 ?; flow rate: 1 ml / min. Baicalin
reference substance for the test product and negative control of the chromatography shown in Figure 1 ~ 3.
2.2 Preparation for the test solution precision the
amount of goods to take this product 1 ml, set 100 ml flask, add the appropriate amount of ethanol, Zhen Yao, ethanol diluted to scale, shake to place filtration, the filtrate
continued to take as a solution for the test items.
2.3 Preparation of reference substance solutions that take precision vacuum dried at 100 ? to constant weight
baicalin reference substance, add ethanol, made from 0.01 mg per ml of solution, as a reference substance solution.
2.4 The linear relationship of the study were drawn
precise concentration of 10 μg / ml of baicalin reference
substance solution 2.0,4.0,6.0,8.0,10.0 μl, injection of
high-performance liquid chromatography to measure the peak area. The results in Table 1.
Figure 1 baicalin HPLC chromatogram of reference
substance (abbreviated)
Figure 2 for the test materials HPLC chromatogram (omitted)
Figure 3-negative samples missing skullcap HPLC chromatogram (omitted)
Table 1 Standard curve of baicalin reference substance
data (omitted)
To the content of baicalin abscissa, baicalin the peak area of the vertical axis drawn standard curve and the data obtained by the regression equation was: y = 0.04x +1 E-16, r
= 0.999 9.
Figure 4 Standard curve of baicalin reference substance
(abbreviated)
Measurement results show that the sample volume of 0.02 ~ 0.10 μg within the sample volume and the peak area linear relationship was good.
2.5 precision inspection precision drawing solution of the above-mentioned reference substance 6 μl, duplicate
sample 5 times. The results in Table 2.
Table 2 precision inspection results (omitted)
The results show that good precision instruments.
2.6 Stability test sample solution taken at 0,2,4,6, and 8 h, respectively sample 1 μl. The results in Table 3.
Table 3 Stability Test Results (abbreviated)
The results showed that the sample for the test solution was stable in the 8 h period.
2.7 Repeatability test method for determination of terms of a formulation on the same batch of samples Samples were prepared for the test solution injection 1 μl, measured peak
area and calculate the content of baicalin, the results shown in Table 4. Reposted elsewhere in the paper for free download http://
Table 4 Repeatability results (omitted)
The results showed that the five test items for the measured values of the relative standard deviation of 1.13%, this law has good repeatability.
2.8 The average recovery experiment to take samples of known content in all three copies of reference substances were added to baicalin solution 5,10,15 ml, according to the above method of sample preparation, preparation for the test materials increases sample recovery solution and injected into high-performance liquid chromatography to calculate recovery. The results in table 5.
Table 5 The average recovery experiment (omitted)
Results show that: The average recovery was 95.8%, RSD
0.87%, this law has good recovery rate.
2.9 Determination of test items taken for the solution method according to the assay, measuring absorbance for the test materials integral value and reference substance absorption integral values calculated for the test materials
in the content of baicalin, that too. The results in table 6.
Table 6 Determination of content of the sample (omitted)
According to measurement results, the tentative Qingrejiedu oral liquid in each (10 ml) contained baicalin not
less than 10 mg.
3 Conclusion
In this study, baicalin as a quantitative indicators, using high performance liquid chromatography Qingrejiedu Oral baicalin contents were determined. The results show that quantitative analysis of their HPLC method is simple, easy, and high sensitivity, good reproducibility can be used in its preparation of baicalin in quantitative analysis.
【References】
[1] State Pharmacopoeia Commission. Chinese Pharmacopoeia, ? Department of [S]. Beijing: Chemical
Industry Press, 2005:619.
[2] Zhu Shan-yin, ZHANG Guan Shun, ZHAO Ya-doubt, and so
on. Qingrejiedu Oral baicalin and efficient quantitative method to improve gas chromatography [J]. Jiangxi Journal of Traditional Chinese Medicine, 2004,16 (4): 46. Reposted
elsewhere in the Free Paper Download Center http://