Compound Qishe tablets quality standard_4212

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Compound Qishe tablets quality standard_4212

Compound Qishe tablets quality standard

     Author: Zhang Yu-quan, Liu Xinhua, Zhang Ning, Liu


    [Abstract] Objective To establish the quality standards of the preparation. Methods The thin-layer chromatography musk ketone, acid and qualitative research; using HPLC-ELSD determination of astragaloside. The results in thin-layer chromatography

    in the detection of artificial musk and artificial bezoar; astragaloside in the 5.175 ~

    36.225 μ g showed good linear relationship within the framework of, r = 0.999 9, plus sample average recovery was 98.66%, RSD of 1.99%. CONCLUSION The method is simple, specific, reproducible, can be used as compound Qishe quality control of tablets.

    [Key words] compound Qishe tablets Astragaloside quality standards

     Abstract: ObjectiveTo establish a quality control for Compound Qishe tablets. MethodsMoschus artifactus and Calcucus bovis artifactus were identified by TLC, and astragaloside IV in the tablets was determined by HPLC-ELSD. ResultsThe spots in the

    TLC were clear and distinguished well.The linear range was within the range of 5.175 ~ 36.225μ g (r = 0.999 9). The average recovery was 98.66%, and the RSD was 1.99%. ConclusionThis methods can be used for quality control of Compound Qishe tablets.

     Key words: Compound Qishe tablets; Astragaloside ? ; Quality control

     Compound Qishe film is Chinese herbal compound preparation, with Qi stasis, dampness Tongluo, swelling analgesic effect. Prescription from Astragalus, artificial

    musk, artificial bezoar and so the composition of Medicine Smell. Reference to 'drug registration management methods' technical requirements, right through the clinical use of proven effective prescription drug side compound Qishe Pharmaceutical

    Research the completion of the preparation process on the basis of the study, using modern analytical techniques and methods to study the establishment of the preparation quality standards. Thin-layer chromatography were used (TLC) on the

    preparation of musk, artificial bezoar for identification. Astragalus in this recipe as a monarch herb, its characteristic ingredients of Astragaloside. ''1995 Edition and the Chinese Pharmacopoeia 2000 edition of astragalus have received under the assay

    contains a thin-layer chromatography astragaloside content, the 2005 edition of' Chinese Pharmacopoeia 'income contained in the HPLC method for the determination of [1]. Since the preparation of compound preparation, the composition of the structure

    belongs to Astragalus saponins [2], weak absorption in the ultraviolet region, using HPLC determination of the use of evaporative light scattering detector for testing to ensure the quality of preparations.

     An instrument and reagent

     1.1 Instrument

     HP-1100HPLC the U.S. Hewlett-Packard; PL1000 Evaporative Light Scattering


     1.2 Astragaloside drug test drugs and biological products in China provides for the determination of use; batch 0781-9706; musk ketone, acid of Pharmaceutical and

    Biological Products are provided for identification purposes; acetonitrile HPLC pure, water filtration re-distilled water and the remaining reagents were analytical pure.

     1.3 Drug compound Qishe film, produced by the Shanghai Traditional Chinese

    Medicine Pharmaceutical Factory, batch number 000315,000325,000330.

     2 Methods

     2.1 TLC

     2.1.1 Identification of musk to take this product 15 g, small study, plus ethyl ether -

    acetone (4:1) 25 ml ultrasonic extraction 15 min, filtration, the filtrate natural Hui dry ethyl 1 ml vinegar residue allows the dissolved, As a solution for the test items. Muscone an alternative reference substance made from vinegar Ethyl 2 μ g per ml of solution, as a reference substance solution. According to thin-layer chromatography

    ( 'The 2005 edition of Chinese Pharmacopoeia Appendix ? Department YI B)

    experiment, to learn for the test product solution, 3 μ l, reference substance solution, 5μ l, respectively, points on the same silica gel G thin-layer board with toluene as the

    mobile phase, started, dried, sprayed with dinitrophenylhydrazine test solution. Test products for chromatography, chromatography with the reference substance for the corresponding position, substantially the same color spots. Figure 1.

     2.1.2 Identification of Artificial Bezoar take this product 4, and research fine, add 5 ml of ethanol ultrasonic treatment 5 min, filtration, filtrate Hui dry residue add 1 ml of ethanol allows the dissolved as a solution for the test items. An alternative bile acid reference substance, add ethanol, made from 1 mg per ml of solution, as a reference substance solution. According to thin-layer chromatography ( 'The 2005 edition of

    Chinese Pharmacopoeia Appendix ? Department YI B) experiment, to learn for the

    test product solution, 3 μ l, reference substance solution, 2 μ l, respectively, points on the same silica gel G thin-layer plate in order to n-hexane - acetic acid Ethyl - glacial

    acetic acid - methanol (20:25:2:3) as the agent, started drying, spray with 10% ethanol solution of sulfuric acid, heated at 105 ? to spot clear set UV lamp (365 nm) under

    review. Test products for chromatography, chromatography with the reference substance for the corresponding position, substantially the same color of the fluorescent spots. Negative control solution without interference. Figure 2. Reposted elsewhere in the paper for free download http://

     2.2 Preparations Astragaloside Determination

     2.2.1 Chromatographic conditions

     Mobile phase: acetonitrile - water (32:68); flow rate 1 ml / min; column

    temperature: 25 ? ; detector conditions: evaporation temperature: 100 ? ,

    vaporization temperature of 80 ? , gas flow rate of 1.5 L / min. Column C18 (250 mm *

    4.6 mm, 5 μ m)

     2.2.2 System suitability test

     Preparation for the test product solution, to take the test materials for the solution of 20 μ l injection of high-performance liquid chromatograph, astragaloside retention time of about 12 min, the number of theoretical plates Astragaloside account in accordance with no less than 4500.

     2.2.3 linear relationship between the study

     Astragaloside take appropriate reference substance, precision, said set, plus methanol made from 1 mg per ml of solution, shake, that is, too. The reference substances were drawn into the sample solution, 5,10,15,20,25,30, and 35μ l of the chromatographic conditions developed in accordance with the determination of peak area was to sample the amount of the natural logarithm of the horizontal axis, the natural logarithm of peak area Ordinate, linear regression, regression equation Y = 1.621 6X 3.281 5, r = 0.999 9, shows that astragaloside 5 .175 ~ 36.225 μ g in the context of a good linear relationship.

     2.2.4 precision experiments on the same test materials for the determination of solution according to the law five times, RSD = 0.49%, results show into the kind of precision and precision instruments are good. Table 1. Precision of experimental results

    in Table 1 (omitted)

     2.2.5 Repeatability test for test products to take the same batch number five copies, according to assay conditions of operation and to determine, RSD = 1.32%, showed good reproducibility and the operation results in Table 2. Table 2 Repeatability

    results (omitted)

     2.2.6 stability test will be a solution for the determination of test items after a certain time interval and then repeat the injection determination, RSD = 0.49%, results show that the tested materials was stable solution at 6 h results in Table 3. Table 3 Stability test results (omitted)

     2.2.7 Experimental and accurately the amount of recoveries obtained Astragaloside reference substance added to the known content of the tested products

    (batch of 000,325), in accordance with determination of the body under the operation and measurement results in Table 4. Table 4 Determination results of recovery


     Recovery (%)=( Astragaloside measured the amount - the amount of known

    Astragaloside) by adding the amount Astragaloside * 100%

     2.2.8 Determination of the tested materials research detailed in this product, take 1.5 g, precision, said determined set Soxhlet extractor, add methanol 40 ml, cold soak overnight, combined with an appropriate methanol, reflux 4 h, recovery of methanol extract and concentrated to the dry residue 10 ml water fever allows the dissolved, extracted two times with ether Zhen Yao, 10 ml / second, abandoned to the ether solution with water saturated n-butanol extract Zhenyao 4 times (20,20,20,10 ml ), n-

    butanol extract combined with ammonia test solution was extracted two times, 20 ml / second, abandoned to the ammonia solution, n-butanol liquid evaporated and the

    residue dissolved in methanol plus 2 ml volume and transferred to a bottle, add

    methanol to the scale, shake, as a solution for the test items.

     Precision reference substance solution were drawn with different batches of test products for the solution of 20μ l, into the liquid chromatograph, which was measured.

    Determination of the three approved agents results in Table 5. Table 5 Determination results (omitted)

     Measured from the preliminary findings of the three groups to determine content in compound preparations Qishe tablets each containing Astragaloside about 0.15 mg.

     3 Discussion

     In this study, test materials for the preparation of solution with reference to 'The 2005 edition of Chinese Pharmacopoeia ? under the Ministry of Astragalus

    astragaloside test products for the determination of solution preparation method. Medicine Smell in order to avoid the interference of other prescription, in the n-

    butanol increased the ether before the extraction steps to remove the interference of fat-soluble components of the test, verified by experiment in the non-ether extract

    Astragaloside components exist; Pharmacopoeia of the extract is also used by macroporous resin column purification method, but to be tested for fear of the ingredients are adsorbed to affect the recovery rate, thus, the experimental operation of this step was omitted. The experimental results show that the test operation can achieve the desired separation.


     [1] State Pharmacopoeia Commission. Chinese Pharmacopoeia, ? Department

    of [S]. Beijing: Chemical Industry Press, 2005:212.

     [2] Yang Yun, Feng health. Extraction and separation of chemical constituents of traditional Chinese medicine handbook [M]. Beijing: China Traditional Chinese Medicine Press, 1998:302. Reposted elsewhere in the paper for free download http://

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