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And stomach pain tablets quality standard of_4014

By Ronald Matthews,2014-10-30 09:23
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And stomach pain tablets quality standard of_4014

And stomach pain tablets quality standard of

    [Abstract] Objective To establish and stomach pain tablets quality standards. Methods using high performance liquid chromatography of berberine hydrochloride medicine Fang Coptis (C20H17NO4 * HCl) content. And the same time, Coptis chinensis,

    Corydalis, costas carried out by TLC. Results Determination of berberine hydrochloride injection volume of 0.085 ~ 0.850μ g good linearity, r = 0.999 9, the average recovery of 96.7%, RSD of 1.53%. TLC qualitative identification of negative

    non-interference, reference substance for the test items with the neat solution of the corresponding spots and clear. Conclusion The detection approach is convenient, accurate, reproducible, and can be used for the preparation of quality control.

    [Key words] and stomach pain tablets; TLC; high-performance liquid

    chromatography; berberine hydrochloride

     Abstract: Objective To establish the quality standard for Heweizhitong tablet. MethodsThe content of Rhizoma coptidis (berberine hydrochloride) in Heweizhitong

    tablet was determined by HPLC. Rhizoma coptidis, Rhizoma corydalis, banksian rose were identified by TLC. ResultsBerberine hydrochloride showed a good linearity in the concentration of 1.03 to 5.15μ g, r = 0.999 93, the average recovery rate was 96.70%

    and the RSD was 1.53%. The TLC blank test showed no interference and theTLC spots developed were fairly clear. ConclusionThe method is simple, accurate and reproducible, and it can be used for the quality control of Heweizhitong tablet.

     Key words: Heweizhitong tablet; TLC; HPLC; Berberine hydrochloride

     And stomach pain tablets income is contained in the 'compilation of the national standards for proprietary Chinese medicines, Chinese patent medicines increased the

    national standard part of the local standards', by Dahongpao, chicken Yafuji, Guan Zhong, Jin buckwheat, berberine, Amomum villosum, Corydalis, costas composed of eight medicinal taste. Indication Yi medicine: guess Niger Wai fast, Wai nisos; Chinese

    medicine: Qi and blood circulation, and stomach pain. For hepatogastric Qi stagnation, Damp-heat deposition due to acute and chronic resistance gastroenteritis, gastric and duodenal ulcers, chronic colitis. And stomach pain tablets in the treatment of

    proprietary Chinese medicine for these diseases, the market demand is strong. In order to control the quality of the other authors of Coptis chinensis, Corydalis, costas for TLC, high performance liquid chromatography of berberine in Coptis by HPLC was

    studied.

     An instrument and reagent

     1.1 Instrument

     Agilent G1311A Quat Pump, G1314A VWD, G1379A DEGASSER, AT-330

    column temperature box, Xtema Rp18 (150 mm * 3.9 mm, 5 μ m) column, Sartorius automatic electronic balance (Sartorius, Germany).

     1.2 reagent silica gel G (Qingdao Marine Chemical Plant); chromatography pure acetonitrile; other reagents were of analytical grade; berberine hydrochloride reference substance (China Pharmaceutical and Biological Products offered by numbered

    110713-200208, in order for the determination of use) ; tetrahydropalmatine reference substance (China Pharmaceutical and Biological Products laboratory provided Tetrahydropalmatine reference substance Lot :110726-200208, for the qualitative

    determination of use); and stomach pain tablets sample (homemade).

     2 Methods and Results

     2.1 Qualitative Identification of

     2.1.1 Coptis by TLC [1]

     To take this product 25, and research fine, plus 1.5 ml of ammonia test solution to

    wet, add chloroform 30 ml, ultrasonic treatment 15 min, filtration, the filtrate evaporated and the residue add 1 ml of methanol allows the dissolved, as a test for product solution. Coptis an alternative medicine 0.5 g in control and non-prescription

    medicines berberine-negative samples made according to preparation method, in

    contrast with the legal system, medicine solution. According to thin-layer

    chromatography experiments, learn from the above-mentioned three kinds of solutions

    of 2μ l, respectively, at the same point with sodium carboxymethyl cellulose as a binder of silica gel G thin-layer plate, n-butanol - acetic acid - water (7:1 : 2) as the agent,

    started out, drying, home ultra-violet light (365 nm) under review. Test products for

    chromatography, in and control the corresponding position medicinal

    chromatography, Hin same color fluorescent spots. Negative control without interference. Figure 1.

     2.1.2 Corydalis by TLC [2]

     To take this product 50, and research fine, plus methanol 50 ml, ultrasonic

    treatment 15 min, filtration, the filtrate evaporated and the residue add 20 ml of water allows the dissolved, with concentrated ammonia test solution to adjust pH value of 8 ~ 10, using ether vibration Shake extracted three times, 15 ml / second, the merger ether

    fluid, evaporated and the residue add 1 ml of methanol allows the dissolved, as a solution for the test items. Take tetrahydropalmatine reference substance, add methanol made from 1 mg per ml of solution, as a reference substance solution.

    Another take prescription medicines without dl-negative samples made according to

    preparation method, and then for the Preparation of test solution, made of materials with negative sample solution. According to thin-layer chromatography experiments,

    learn from the above-mentioned three kinds of solution of 5 μ l, respectively, at the same point with sodium carboxymethyl cellulose as a binder of silica gel G thin-layer

    board with toluene - acetone (9:2) as the agent , started out, dried, smoked home iodine

    vapor to spot color definition. Daylight view for the test materials chromatography, chromatography with the reference substance for the corresponding position, substantially the same color of the spots; waving in the air board to do the iodine

    adsorption, the home UV light (365 nm), under review for Test items chromatography, chromatography with the reference substance for the corresponding position, substantially the same color of the fluorescent spots. Negative control without interference. Figure 2. Reposted elsewhere in the paper for free download http://

     2.1.3 Muxiang by TLC

     To take this product 10, and research fine, plus chloroform 10 ml, ultrasonic treatment 30 min, filtration, the filtrate concentrated to 1 ml, as a solution for the test

    items. Take Dehydrocostus lactone and costunolide appropriate reference substance, add methanol produced each containing 0.5 mg per ml of mixed solution as a reference substance solution. An alternative non-prescription medicines wood made negative by

    preparation method and then the sample preparation method for the solution of test items made negative sample solution. According to thin-layer chromatography test,

    drawing the above-mentioned three kinds of solution of 5 μ l, respectively, at the same

    point with sodium carboxymethyl cellulose as a binder of silica gel G thin-layer plate in

    order to chloroform - cyclohexane (5:1 ) as the agent, started out, dried, sprayed with anisaldehyde test solution, heated at 105 ? to spot color clarity. Test products for

    chromatography, chromatography with the reference substance for the corresponding position, substantially the same color spots. Negative control without interference. Figure 3.

     2.2 Determination

     2.2.1 Preparation of reference substance solution precision Weigh 5 h drying at 100 ? for the amount of berberine hydrochloride reference substance, add methanol produced per ml containing 60 μ g of berberine hydrochloride in the solution, filtration derived.

     2.2.2 Preparation for the test product solution [3] to take this product 10, except for coating, and research fine, take about 0.5 g, precision that set, and placing a plug taper bottle, adding 80% methanol-precision 25 ml, Mesa, said that given the weight,

    ultrasound treatment (power 90 W, frequency 59 kHz) 40 min, remove and let cool and then said that given the weight reduction with 80% methanol to complement the weight loss, shaking, filtration, take added filtrate, derived.

     2.2.3 Chromatographic conditions and experimental results Column: Xtema Rp18

(150 mm * 3.9 mm, 5 μ m); column temperature: 30 ? ; mobile phase: acetonitrile -

    0.1% phosphoric acid (40:60) (each 100 ml plus 10 2 alkyl sulfonate 0.1 g); detection wavelength 265 nm; flow rate 1 ml / min, do the same condition analysis, preparation of berberine hydrochloride and other components of the peak can reach the baseline separation. Reference substance solution for the test product solutions and lack of negative reference substance berberine solution chromatogram. Figure 4 ~ 6.

     2.2.4 Precision linear range of the study, said taking berberine hydrochloride reference substance 17.0mg, Liang Ping set 25 ml, add 80% methanol solution allows the dissolved and diluted to the scale, shake (concentration of 680 μ g / ml) , and then

    draw reference substance were precise amount of mother liquor, with 80% methanol solution diluted to different concentrations of reference substance solution: 17.0,34.0,68.0,85.0,170.0 μ g / ml. Respectively, the precise drawing of the reference

    substance solutions of different concentrations of 5 μ l, according to the body of the chromatographic conditions for analysis of injection to peak area value of the vertical axis, the amount of berberine standard curve drawn for the abscissa (Figure 7),

    calculate Berberine regression equation was: Y = 3 685.126 28X 15.652 020 17, r = 0.999 93. That berberine hydrochloride injection volume 0.085 ~ 0.850 μ g good linear relationship within the scope.

     2.2.5 Experimental precision precision drawing solution of berberine

    hydrochloride reference substance (68.0 μ g / ml) 5 μ l, repeat sampling five times, according to the above chromatographic conditions were measured peak area. In order to seek the relative standard deviation of berberine hydrochloride in the value of total peak area RSD of 0.54%. Showed good precision instruments.

     2.2.6 reproduce the experiment were collected from the same batch (20,051,001), and stomach samples of five copies of painkillers, according to the body of the method

    of determination under the experiment measured the content of berberine hydrochloride. Berberine content in the sample relative standard deviation of 0.57%, indicating good reproducibility of this method.

     2.2.7 stability test to take under the above-mentioned standard curve solution of

    berberine hydrochloride reference substance (68.0 μ g / ml), and stomach and painkillers for the solution of the test product 5 μ l, respectively, 0,2,4,6,8 , 12 injection, according to the body of the determination of conditions under the measured reference substance for the test materials in the 0 ~ 12 h in the peak area RSD were 0.76%, 0.81%, indicating that reference substance for the test materials placed 12 h in the basic stable.

     2.2.8 recoveries obtained experimental precision that berberine hydrochloride reference substance (100 ? drying 5 h) 15.4 mg, Liang Ping set 10 ml, add 80%

    methanol allows the dissolved and diluted to the scale, shake, made of (1.54 mg / ml)

    reference substance solution. Take the same batch (20,051,001) of known concentration and stomach pain tablets (5.79 mg / g) take samples of precision that all five copies, each of about 0.25 g, respectively, by adding the above-mentioned precise solution of

    berberine hydrochloride reference substance of 1 ml, according to Determination of the body were measured under the test items for the solution and determine its content of berberine hydrochloride. The average recovery was 96.7%, relative standard deviation

    is 1.53%, indicating good recovery of this method. The results in Table 1. Table 1 The average recovery results (omitted)

     2.2.9 Determination of content of the sample taken 10 batches of this product, according to the text were determined under assay. The results in Table 2. Table 210

    batches and samples of stomach pain tablets assay results (omitted)

     3 Discussion

     Experiments during the course of berberine hydrochloride reference substance for 80% of the methanol solution to stop pump scanning wavelength range 190 nm to 400

    nm. The results of berberine hydrochloride by ultraviolet characteristic absorption maximum 265 nm, detected at 265 nm due to the system easy to stability and good peak shape in response to large, established for the detection wavelength 265 nm.

     As different origin and harvest time causes of berberine in Coptis medicinal content of high and low, combined with more than 10 batches of samples in the determination of berberine hydrochloride in results, this product content of berberine

    hydrochloride in Each set contains berberine to berberine, this should be not less than 0.70 mg.

[References]

     [1] Yu Xiaoting, fortunately, Huang Hung-wen. And stomach pain capsule

    quality standard [J]. Zhongnan Pharmaceutical, 2004,2 (5): 291.

     [2] PIAO Hui-shan, Shen Hai, ZHENG Yun-hua, et al. UV spectrophotometry off

    the herb compound preparation Tetrahydropalmatine content [J]. Yanbian Medical Journal, 1996,19 (1): 11.

     [3] National Pharmacopoeia Committee. Chinese Pharmacopoeia, ? Department

    of [S]. Beijing: Chemical Industry Press, 2005:213, Appendix VIB. Reposted elsewhere in the paper for free download http://

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