High Performance Liquid Chromatography Card calcium compound content of carbamazepine capsules Iris
Author: Fu Pingping, Jing Hao Ran, ZHAO Zhi-wei
【Abstract】 Objective To establish a calcium compound card iris carbamazepine capsule by high performance liquid chromatography. Methods C18 (200 mm × 4.6 mm, 5 μm) column
with methanol 0.02 mol / L potassium dihydrogen phosphate solution (60:40) as mobile phase. The detection wavelength was 285 nm, flow rate of 1.0 ml / min. Results carbamazepine 0.008 648 ~ 0.172 96 μg peak area was within the range of a good linear relationship (r = 1.000 0, n = 9), the average recovery was 101.44%, (n = 9), RSD 0.49% . Conclusion The method is fast, simple, accurate and can be used for calcium compound
cards iris capsule quality control.
Key words calcium compound card iris capsules; high-
performance liquid chromatography; Carbamazepine; assay
Abstract: ObjectiveTo establish an HPLC method for the determination of Carbamazepine in Compound Kagai Changpu
Capsules.MethodsAn HPLC assay was developed. Chromatographic assay was performed on a column of Hypersil C18 (200 mm × 4.6
mm, 5 μm), using methanol-0.02 mol / L KH2PO4 (60:40) as the
mobile phase with the flow rate of 1.0 ml / min.The detection
wavelength was at 285 nm.20 μl sample and external method
were used.ResultsA satisfactory separation was obtained.The calibration curve was linear over the range of 0.008 648 ~ 0.172 96 μg for ribavirin (r = 1.000 0, n = 9). The average
recovery of ribavirin was 101.44% (n = 9) with RSD of 0.49%. ConclusionThe method is quick and simple with good
reproducibility.It can be used for the quality control of Compound Kagai Changpu Capsules.
Key words: Compound Kagai Changpu Capsules; HPLC;
Carbamazepine; Content detemination
Iris Card calcium compound capsule is Baoding Shichen epilepsy hospital homemade preparations, mainly carbamazepine, calcium hydrogen phosphate, Shichangpu, Schisandra, etc. composed of eight kinds of drugs, the drug has a strong
antiepileptic effect applicable to all types of epilepsy,
psychomotor epilepsy effect is particularly noteworthy. Carbamazepine is a prescription drug in one of the main "Chinese Pharmacopoeia" in 2005 edition of the Department ?
[1] using ultraviolet spectrophotometry carbamazepine content
not suitable for the determination of the compound preparation; also reported the application of HPLC,
methanol and acetonitrile acetic acid solution as mobile phase, Determination of Carbamazepine Tablets [2]. To control the quality of the preparation, this paper adopts high-
performance liquid chromatography with methanol potassium
dihydrogen phosphate solution as the mobile phase was determined by the content of compound preparation of carbamazepine. Are reported below.
An instrument and reagent
Aglient 1100 high-performance liquid chromatography; G1311A quaternary pump, G1313A autosampler, DAD detector (G1315B), ChemStationA.10.01 ChemStation; TU 1810S UV-
visible spectrophotometer (Beijing General Instrument & Poor's analysis of limited liability company ).
Carbamazepine reference substance (China provided medicines and biological products); compound Card calcium grass Pu Capsule (Baoding Shichen epilepsy hospitals); methanol chromatography pure; other reagents of analytical
grade.
2 Methods and Results
2.1 Chromatographic conditions Column: Hypersil BDS (200 mm × 4.6 mm, 5 μm); mobile phase: methanol -0.02 mol / L
potassium dihydrogen phosphate solution (60:40); detection
wavelength: 285 nm; flow rate: 1.0 ml / min; injection volume: 20 μl; room temperature sample. Theoretical plate numbers calculated according to peak carbamazepine should not be less than 2 000. Negative control solution chromatograms show that the peak position carbamazepine peak without interference. Figure 1.
2.2 Preparation of Solution
2.2.1 Preparation of reference substance solution precision Weigh 105 ? drying 2 h carbamazepine reference
substances 0.010 81 g, set 250 ml Liang Ping, add methanol dissolved and diluted to the scale, shake, as a reference substance reserve liquid; precise amount of reserve fluid obtained 5 ml, set in 50 ml Liang Ping, with the mobile phase was diluted to scale, shake, as a reference substance solution. Reposted elsewhere in the paper for free download http://
2.2.2 Preparation for the test product solution were collected from three batches of samples of all 20 will be mixing the contents, and research fine, fine, said appropriate amount (about the equivalent of carbamazepine 10 mg), set in
250 ml Liang Ping, add Methanol dissolved and diluted to the scale, shake, filtration, precision continued to take the amount of filtrate 5 ml, set in 50 ml Liang Ping, with the mobile phase diluted to the scale, shake, as a solution for the test items.
2.2.3 Preparation of negative control solution ratio of 0.25 according to prescription volume, said Fang to take In addition to other drugs than carbamazepine and accessories, and placing 250 ml Liang Ping, the use of methanol diluted to
scale, as a negative control reserve liquid; precision take the amount of 5 ml, set in 50 ml Liang Ping, diluted to scale with the mobile phase, shake, as a negative control solution.
2.3 A methodological survey
2.3.1 linear relationship between the study said that
taking reference substance precision reserve liquid 5 ml, set in 50 ml Liang Ping, diluted with the mobile phase to scale (made with carbamazepine per ml, approximately 4 μg of the
solution), shake ; precise amount of each check
2,5,10,15,20,25,30,35,40 μl, into the liquid chromatograph,
record the peak area. In order to sample volume (μg) as the
abscissa, the corresponding peak area of the vertical axis, linear regression. Results 0.008 648 ~ 0.172 96 μg context,
carbamazepine sample volume and the peak area showed good linear relationship, regression equation Y = 2 830.86X-0.777
46, the correlation coefficient r = 1.000 0.
2.3.2 to 2.2.1 under the experimental precision of the reference substance solution repeated injection six times,
obtained peak area RSD of 0.51% (n = 6), shows a better precision of this method.
2.3.3 stability test to take the same test items for the solution, 0,1,2,4,8 h, respectively, injection 20 μl,
recorded peak area. The results of peak area remained
basically unchanged, RSD is 0.37% (n = 5), showed that at least 8 h for the test solution to stabilize.
2.3.4 Repeatability precision experiments that take five copies of the same batch of samples were determined according to the sample under the method of measuring the average level of 96.76% obtained, calculate RSD = 0.85% (n = 5), shows this method is good reproducibility.
2.3.5 Experimental precision the amount of recovery to take reference substance reserve liquid 4,5,6 ml, Liang Ping
set 50 ml of the respective negative control precision by adding reserve liquid 5 ml, diluted to scale with the mobile phase, injection liquid chromatography record peak area. The results in Table 1. Recovery of experimental results in Table 1 (omitted)
2.4 The content of the sample obtained by determination of items 2.2.1 and 2.2.2 of the reference substance solution and prepared for the test product solution, respectively, injection 20 μl, record peak area to calculate concentration. The results in Table 2. Table 2 Determination of Sample
Results (abbreviated)
3 Discussion
3.1 Determination of detection wavelength for the test materials in the peaks of carbamazepine detected by DAD at 285 nm wavelength of maximum absorption, their uv spectra and uv
spectra of carbamazepine reference substance exactly the same, so choose 285 nm as detection wavelength.
3.2 The method is simple, reliable, easy to operate, good reproducibility and can be used as iris capsules calcium compound cards effective method of quality control.
【References】
[1] State Pharmacopoeia Commission. Chinese
Pharmacopoeia, ? Department of [S]. Beijing: Chemical
Industry Press, 2005:101.
[2] Yu-Xiang Zhao, Song 1, Li Sha Ching. HPLC
Determination of Carbamazepine Tablets [J]. China
Pharmaceutical, 2003,17 (12): 762. Reposted elsewhere in the paper for free download http://www.hi138. com