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High Performance Liquid Chromatography Gengnianle Icariin Capsules_572

By Johnny Robinson,2014-10-30 19:28
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High Performance Liquid Chromatography Gengnianle Icariin Capsules_572

    High Performance Liquid Chromatography Gengnianle Icariin Capsules

     Abstract Objective To establish Gengnianle capsule method for determination of icariin. Methods using high performance liquid chromatography with C18 column (5 μm, 4.6mm × 200

    mm); acetonitrile: water (30:70) as mobile phase; flow rate of 1.0 ml / min, detection wavelength 270 nm. The results of icariin in the range of 0.204 ~ 0.816 μg showed a good linear

    relationship within, r = 0.999 9. The average recovery was

    98.77%, RSD 1.58%. Conclusion The method is simple, sensitive and can be used Icariin gengnianle capsules by HPLC.

     Key words gengnianle capsules; icariin; high-performance

    liquid chromatography

     Abstract: ObjectiveTo establish HPLC method for the

    determination of Icariine in Gengnianle Capsule. Methods LUNA ODS C18 BDS (200 mm × 4.6 mm) was used with acetonitrile

    water (30:70) as a mobile phase. The flow rate was 1.0 ml * min -1. The detecting wavelength was 270 nm. ResultsThe linear range of Icariine was 0.201 ~ 0.816 μg, r = 0.999 9. The

    average recovery was 98.77%. Conclusion The method is simple, rapid and accurate.

     Key words: Gengnianle Capsule; Icariine; HPLC

     Gengnianle capsules from epimedium, oysters, Anemarrhena,

    Rosa laevigata, cork, plantain seed, ginseng etc., with Yang Xin Yang Shen, regulate and fortify the Chong and Ren

    function. Menopause occurs for the night sleep soundly anxiety, palpitations, tinnitus, suspicious sentimental, Hongre sweating, irritability irritability, back pain

    embolism. According to Fang composition, to choose their primary drug of Epimedium icariin content in the control of a target, using high performance liquid chromatography preparation of icariin. Are reported below.

     An instrument and reagent

     HP1100 high performance liquid chromatography, VWD UV detector, HP ChemStation. Column: LUNA ODS C18 column (200 mm × 4.6 mm, 5 μm); ultrasonic extractor (AS3120B).

     Icariin reference substance, purchased in China's

    pharmaceutical and biological products (determination of use, lot number 0737-200011).

     Acetonitrile, methanol for chromatography pure; water as a sub-boiling distilled water; other reagents used were of analytical grade. Gengnianle capsules, self-control, batch

    041.02 thousand; 041,022; 041,025.

     2 Methods and Results

     2.1 The chromatographic conditions were column for the analytical column LUNA ODS C18 column (200 mm × 4.6 mm, 5 μ

    m); mobile phase [1] To acetonitrile: water (30:70); detection wavelength 270 nm; flow rate of 1.0 ml / min; injection volume was 10 μl. Under the above chromatographic conditions separation of icariin and other ingredients well, and the blank solution without interference, shown in Figure 1 ~ 3.

     2.2 Preparation of reference substance solution icariin take appropriate reference substance, precision, said set, plus methanol produced per ml solution of 50 μg of icariin,

    that was.

     2.3 Preparation of solution for the test materials [2] to take the contents of the product powder (over 80 mesh sieve) about 2.0 g, precision that set, and placing 100 ml bottle with cone-shaped plug, precision by adding 50% ethanol 50 ml, density Sierra Leone, saying that given the weight, ultrasound treatment 30 min, let cool, fill with 50% ethanol by weight loss, shaking, microporous membrane (0.45 μm) filtration, the

    filtrate continued to take that too.

     2.4 Preparation of blank solution composed by prescription, to take except Epimedium remaining outside the drug preparation process requests made by non-normal control

    of Epimedium samples prepared according to the tested products were prepared under the blank solution, respectively, draw a blank solution and for the test materials into the liquid chromatograph 10 μl. The results showed that the blank

    solution and for the test product compared to the corresponding location is not a peak that no interference.

     Figure 1 reference substance for HPLC diagram (omitted)

     Figure 2 for the test chemicals HPLC diagram (omitted)

     2.5 linear relationship between the inspection precision weighing icariin standard 5.1 mg buy 100 ml Liang Ping, add methanol dissolved and diluted to the scale, shake, that is,

    too. Precision drawing reference substance solution were 4,6,8,12,16 μl, according to the above chromatographic conditions were injected into liquid chromatograph, record the peak area to peak area values (A) for the longitudinal coordinates, icariin into sample volume (C) as the abscissa, mapping the standard curve regression equation was A = 4164.7C-29.352, r = 0.999 9. Showed that icariin in the range of 0.204 ~ 0.816 μg showed a good linear relationship within. Reposted elsewhere in the paper for free download http://

     Figure 3 blank samples HPLC diagram (omitted)

     2.6 precision experimental precision drawing icariin reference substance solution 10 μl, sample 5 consecutive

    times, the measured peak area average of 1 779, RSD is 1.35%.

     2.7 Repeatability test for test items according to the above solution preparation method, saying that obtained with

    the batch sample (Lot 041.02 thousand) 5 copies, respectively, were measured. Icariin was the average content 0.33 mg / tablets, RSD 1.36%.

     2.8 stability test to take the same test materials for the solution (batch 041.02 thousand), respectively, 0,2,4,8,12 h after preparation according to the determination of peak area average of 1522, RSD is 2.28%, indicating that the sample solution at 12 h to stabilize.

     2.9 recovery experiment to increase sample recovery method (by adding 1:1), precision levels that are known to take samples of the same batch number (041020) 1.0 g total of five copies, respectively, by adding precise concentration of

    1.1 mg / ml of Epimedium glycoside reference substance solution 1 ml, water bath, evaporated, mixed evenly, according to 2.3 for the test materials were prepared under the solution, precision drawing 10 μl, into the liquid

    chromatograph, the same method. Calculation of the average

    recovery was 98.77%, RSD of 1.58% (n = 5). The results in Table 1.

     Table 1 Experimental results of recovery of icariin (omitted)

     2.10 Determination of the results of samples taken three batches (041020,041022,041025) samples, three samples of each batch, according to the sample solution were extracted under preparation, the results of three batches of samples the average content of icariin were 0.33,0.29,0.33 mg / tablets.

     3 Discussion

     3.1 The mobile phase of election newspaper reference [1,2] were selected methanol: water (62:38), methanol: 0.1 mol / L sodium dihydrogen phosphate-water (52:48), acetonitrile:

    water (30:70 ) as the mobile phase experiments found that acetonitrile: water (30:70) as mobile phase, the measured

    object separation is better, less interference of impurities, so choose it as a mobile phase of this Law.

     3.2 Sample preparation methods have been used 70% ethanol heating reflux extraction and ultrasonic extraction with 50%

    ethanol and found that 50% ethanol, derived from ultrasonic

    extraction of impurities less, the measured component separation is good, and the operation is simple, fast, so choose this Act .

     Experiments show that the assay method is simple and

    reliable, easy to operate, reproducible, this product can be used as an effective method of quality control.

     References

     [1] State Pharmacopoeia Commission. Chinese Pharmacopoeia, ? Department of [S]. Beijing: Chemical

    Industry Press, 2005:545.

     [2] Miao-Ming 3, Zhen-Guo Li. Modern and practical

    medicine quality control techniques [M]. Beijing: People's Health Press, 2000:971. Reposted elsewhere in the paper for free download http://

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