High Performance Liquid Chromatography bile Lichou capsule contents Geniposide_462

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High Performance Liquid Chromatography bile Lichou capsule contents Geniposide_462

    High Performance Liquid Chromatography bile Lichou capsule contents Geniposide

     Author: Fu Yu-hai, ZHANG Li-Sheng, Chang-Ling


     Abstract Objective high-performance liquid chromatography bile Lichou capsule Geniposide content. Method column of

    Kromasil C18 column; mobile phase was methanol water

    (75:25); detection wavelength was 238 nm; flow rate of 1.0 ml * min-1. The results of the linear range of 11.6 ~ 58.0 μg *

    m l-1, r = 0.999 8; the average recovery was 98.95%, RSD of

    0.97%. Conclusion The method is simple, sensitive and accurate.

     Key words high-performance liquid chromatography; bile Lichou capsule; geniposide

     Bile Lichou capsule from gardenia, rhubarb, JGC and other flavor ingredients extracted crafted more than a decade, is in Heihe City, Heilongjiang Province, the First People's Hospital for many years a common hospital preparation (black Wei pharmacists characters [1997025] number). Efficacy Shuganlidan pain, Qingrejiedu RONGSHI. For acute and chronic

    cholecystitis, cholangitis, acalculous cholecystitis and gallstones treatment. Fang Gardenia diuretic heat, cooling blood detoxification, modern pharmacological experiments to prove Geniposide Gardenia in bile flow with the increase in the role of Liver gallbladder. The preparation for the self-

    made side, the original standard-free detection of targets. To

    improve product quality, do something useful to explore, choose Geniposide quantitative indicators as quality control, using high-performance liquid chromatography was determined by its content. Are reported below.

     An instrument and reagent

     1.1 Instrument LC 10ATvp-based high-performance liquid

    chromatography (Shimadzu), SPD 10Avp UV detector

    (Shimadzu), N3000 chromatography workstation (Zhejiang University Intelligent Information Institute).

     1.2 reagent Geniposide (Chinese medicines and biological

    products, 749 200108); bile Lichou capsule (Heihe City, Heilongjiang Province, the First People's Hospital of preparation room, batch number 050512,050821,051208,060304); home-made ultra-pure water ; Methanol HPLC pure.

     2 method [2] and results

     2.1 The chromatographic conditions were mobile phase was methanol water (75:25) [1]; column of octadecyl silane bonded silica packed column; wavelength: 238 nm; flow rate of 1.0 ml * min-1; injection volume 10 μl; column temperature of

    27 ?. Number of theoretical plates should not be accrued by Geniposide less than 1500, with other components of Geniposide separation should meet the requirements.

     2.2 The solution for the test materials prepared by bile Lichou capsule contents 0.3 g, precision that set, and placing a flask in Cyprus, precision by adding methanol, 50 ml, weighing, ultrasound treatment two times, 25 min / times, released after cooling weighing, methanol supplement weight, shaken, centrifuged and the supernatant with 0.45 μm

    microporous membrane filter, spare.

     2.3 Preparation of reference substance solution and the linear relationship between the study said that taking Geniposide precision reference substance 11.6 mg, buy 100 ml Liang Ping, add methanol dissolved and diluted to the scale, shake, as a reserve liquid. Precise amount of take home 1.0,2.0,3.0,4.0,5.0 ml respectively 10 ml Liang Ping, add methanol concentration of the preparation into

    11.6,23.2,34.8,46.4,58.0 μg * ml-1 of the reference substance

    solution, respectively, sample 10μl , the measured peak area,

    the regression equation is A = 33 861C-5 653, r = 0.999 8.

    That Geniposide at 11.6 ~ 58.0 μg * ml-1 range of good

    linearity. Reposted elsewhere in the paper for free download


     2.4 Stability of Reference Substances check store diluted into 29.0 μg * ml-1 solution, according to the above-

    mentioned chromatographic conditions, according to 0,1,2,3,4,5,24 h measured peak area, the measured peak geniposide The average area of 980 241, RSD 1.08%, Geniposide

    24 h in methanol was stable.

     2.5 Blank experiments with the system by prescribing the ratio law, made of non-gardenia samples for the test products in accordance with the rule of law into a system solution blank control solution. Determined according to the law,

    resulting in a peak position Geniposide no other peaks, indicating that under the experimental conditions, and other medicinal ingredients on the determination of no interference. The results shown in Figure 1.

     2.6 precision experiments take "2.4" under the reference substance with a good solution, 10μl / times, repeated

    sampling six times, the measured peak area mean 978915, RSD is 0.83%.

     2.7 Repeatability test for test taking goods (Lot 060,304) contents six copies, each 0.3 g, precision that will, according to "2.2" under the operation, the measured peak area; this product installed capacity of 0.3 g, calculate the average content of 4.29 mg * g-1, the RSD is 1.06%.

     a Geniposide reference substance for the test b

    product c negative control

     Figure 1 Capsules high-performance liquid chromatography

    of bile Lichou (omitted)

     2.8 Weigh a known recovery of experimental precision for the content of test items (Lot 060,304) 6 copies, each 0.15 g,

    cone-shaped bottle home with Sierra Leone, precision by adding the concentration of 116 μg * ml-1 in contrast geniposide

    Commodities reserve liquid 5 ml, Hui dry solvent, according to "2.2" under the "purchase a plug flask, the ... ..." If the method is, by external standard method. The results in Table 1.

     2.9 Determination of the sample taken four batches of samples of 0.3 g, precision that determined according to the law made for the solution of test items, and the other to take Geniposide reference substance, add methanol made from 30 μg

    * ml -1 solution, respectively, drawn for the test product solution and the reference substance solution of 10 μl into

    the column and peak area measured by external standard method to calculate Geniposide content. The results in Table 2.

     Table 1 plus sample recovery results (omitted)

     Table 2 Determination of Sample Results (abbreviated)

     3 Discussion

     4 batch preparation Geniposide determination of the results, which mean 1.26 mg / tablets, taking into account

    such factors as efficacy and extraction, defined as each piece Geniposide content of not less than 1.2 mg is more appropriate.

     Detection of the choice of ingredients, a larger amount of gardenia in the preparations, the gallbladder Geniposide is Gardenia composition, high content, high-performance liquid

    chromatography determination of bile Lichou capsule Geniposide content, method is simple and , accurate, reproducible, in order to nourish the liver capsule quality control of the



     [1] Xiao Pei-Gen. A New Chinese medicine chi, Volume 2 [M]. Beijing: Chemical Industry Press, 2001:476.

     [2] National Pharmacopoeia Committee, Chinese

    Pharmacopoeia, ? Department of [S]. Beijing: Chemical

    Industry Press, 2005:350. Reposted elsewhere in the paper for free download http://

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