6 Ling Detoxification Pills Quality Standards
【Abstract】 Objective To establish a six-ling detoxification
pill quality standards. Methods TLC method bezoar was identified using HPLC determination of Chinese toad venom poisoning and lipid-based ligand content of toad poison. Using ZorbaX C18 column, mobile phase of acetonitrile -0.5%
potassium dihydrogen phosphate solution (35:65) (adjusted with phosphoric acid PH value of 3.2), the detection wavelength was 296 nm. The results of TLC chromatographic spots were clear. Chinese toad venom poisoning based on 0.311 6 ~ 2.492 8 μg
showed a good linear relationship between, fat toad poison ligand at 0.309 6 ~ 2.476 8 μg showed a good linear
relationship between the. Chinese toad venom poisoning the base average recovery of 99.18%, RSD = 1.55%. Fat toad poison ligand average recovery of 103.30%, RSD = 1.73%. Conclusion The method is simple and feasible, reproducible, good for six-
Ling detoxification provides a method of quality control pills.
Key words 6-Ling Wan Chinese toad venom poisoning
detoxification grease toad poison ligand quality standards
Quality Standard for Liulingjiedu Pill
Abstract: ObjectiveTo establish a quality standard for Liulingjiedu pill.Methods Calculus bovis in this medicine was identified by TLC. Cinobufagin and Resibufogenin in
Linlingjiedu pill were determined by HPLC, using Zorbax C18 column and CH3CN: KH2PO4: 35:65 (adjust pH3.2 ) as the mobile phase. The detective wavelength was 296 nm.ResultsThe TLC spots developed were quite clear. Cinobufagin and resibufogenin showed a good linear relationship at a range of 0.3116 ~ 2.492 8 μg and 0.309 6 ~ 2.476 8 μg.The average
recovery of Cinobufagin was 99.18% and RSD was 1.55%. The average recovery of Resibufogenin was 103.30% and RSD was 1.73%. ConclusionThe method can be used for the quality
control of Liulingjiedu pill.
Key words: Liulingjiedu pill; Cinobufagin; Resibufogenin; Quality standard
6 Ling detoxification of Chinese medicine pill for ministerial standards set prescription drug formulations containing relevant species, with a heat-clearing and
detoxifying, reduces swelling, pain effect. Is widely used in clinical throat diseases. Toad for Fong main drug, but also for toxic herbs. In order to better control drug quality, according to the National Drug Standards Plan of Action to
improve quality standards of the relevant requirements, an increase of bezoar by TLC and the Chinese toad venom poisoning based, fat toad poison ligand assay.
An instrument and reagent
AL204 ten thousandth electronic balance (Mettler Inc.);
Agilent1100 high-performance liquid chromatography (Agilent Technologies Inc. USA); KQ 100B ultrasonic cleaner (Kunshan Ultrasonic devices Co., Ltd.); China-based and fat toad toad
venom poisoning toxic ligand standard (purchased in China's Pharmaceutical and Biological Products Institution, lot number 110803 200504 and 0718 9306, for the determination);
acetonitrile, methanol, phosphoric acid for chromatographic purity, potassium dihydrogen phosphate for the analysis of pure.
2 Methods and Results
2.1 Bezoar TLC [1,4] taking this product about 2 g, small
study, set 10 ml Liang Ping, add 10% of the amount of acetic acid ethanol solution, fully Zhen Yao, the 10% acetic acid ethanol solution of constant volume to the scale, put it aside for 24 h, the supernatant solution, as for the test items. Bezoar take control herbs 0.1 g, with the rule of law must control medicinal solution. And then take bile acid reference substance, plus 10% ethanol made from acetic acid containing 1 mg per ml of solution, as a reference substance solution. Apart from Bezoar taken outside the medicine, according to the sample preparation process made from the negative control samples, and then take the negative control sample for the test products in accordance with the preparation method of solution made from the negative control solution, the solution
of the draw 5 μl, respectively, points on the same piece of silicon G TLC plate in order to n-hexane - ethyl acetate -
methanol - acetic acid (6:32:1:1) as the agent, started out, dried, sprayed with 10% phosphomolybdic acid ethanol solution,
105 ? heated to a clear spot. Test products for
chromatography, in HPLC with the control reference substance for medicinal and the corresponding position, substantially the same color of the spots, negative control without interference.
2.2.1 Chromatographic conditions [1 ~ 3] acetonitrile -
0.5% potassium dihydrogen phosphate solution (35:65) (adjusted with phosphoric acid pH = 3.2) as mobile phase; detection wavelength 296 nm; theoretical plate number Toad poisoning by
China-based, fat toad poison ligand peaks were calculated shall not be less than 4000.
2.2.2 Preparation of standard curve precision to take Chinese toad venom poisoning, said the base reference substance amount, plus the concentration of methanol produced
0.155 8 mg / ml solution of the reference substance, respectively, sample 2,4,8,12,16,20 μl. Precision said the
fat toad poison to take appropriate ligand reference
substance, plus the concentration of methanol produced 0.1548 mg / ml solution of the reference substance, respectively, sample 2,4,8,12,16,20 μl. Abscissa with reference substance concentration, peak area value of the vertical axis and draw into a working curve, calculated base Chinese toad venom poisoning regression equation: y = 771x 30 (r = 0.999 9), fat
toad poison regression equation of the ligand : y = 794.6x-
10.1 (r = 0.999 9). The results showed that the base in the Chinese toad venom poisoning 0.311 6 ~ 2.492 8 μg showed a
good linear relationship between, fat toad poison ligand at
0.309 6 ~ 2.476 8 μg showed a good linear relationship
between the. Reposted elsewhere in the paper for free download http://
2.2.3 Preparation for the test product solution to take samples of about six-Ling detoxification pills 90 mg,
precision that set, and placing a plug conical bottle, precision adding methanol 10 ml, said that given the weight, ultrasound treatment 50 min (power 250W, frequency of 40 kHz), let cool, and then said that given the weight by using methanol to complement the weight loss, shaking, filtration, take added filtrate that was.
2.2.4 Experimental get the same precision for the test product solution into the sample measured 6 times, respectively, Chinese toad venom poisoning the base peak area RSD values of 0.62%, fat toad poison ligand peak area value of the RSD was 0.95%, indicating that Instruments have a good precision.
2.2.5 repeated experiment to take the same group of 6 samples of six copies of spiritual detoxification pills, according to test products for the solution preparation
methods dealt with separately, determined Chinese toad venom poisoning and lipid-based ligand toad poison, the average
total content of 12.0116 mg / g, RSD of 1.69%. The results showed good repeatability. 2.2.6 stability test to take the
same sample solution, respectively, 0,1,2,4,8,12 h determination of content of the sample of RSD = 0.83%. Samples showed that 12 h to stabilize.
2.2.7 The average recovery experiment with adding sample collection method, taking the known Chinese toad venom
poisoning poisonous toad-based and lipid content of six ligand Spirit detoxification Pills (Chinese toad venom poisoning poisonous toad-based and lipid ligand contents were 5.804 3 mg / g and 6.207 2 mg / g) 6 copies, each of about 50 mg,
sophisticated set that were added 2 ml Chinese toad venom poisoning and lipid-based ligand toad poison mixed reference substance solution (concentrations were 0.152 9 mg / ml, and 0.145 8 mg / ml), placed in 10 ml flask, add methanol to the scale constant volume, ultrasound treatment (power 250W, frequency 40 kHz) 40 min, let cool, constant volume with methanol to the scale, filtration, whichever Continued filtrate, respectively, injection 20 μl, in calculating the
rates. Chinese toad venom poisoning the base average recovery of 99.18%, RSD = 1.55%; fat toad poison ligand average recovery of 103.30%, RSD = 1.73%. The results shown in Table 1 ~ 2. Table 1 China-based recovery of toad venom poisoning experimental results (slightly) Table 2 fat toad poison
recovery of experimental results with the base (omitted)
2.2.8 Determination of content of the sample to take samples of about 6 Ling detoxification pills 90 mg, precision that set, and placing a plug conical bottle, sophisticated mobile phase by adding 10 ml, said the fixed weight, shake, ultrasound treatment 4 min (power 250W , frequency 40 kHz), released after cooling, then that set the weight by using methanol to complement the weight loss, shaking, filtration, take added filtrate, injection 20 μl.
With the above conditions are determined by three groups of six spiritual detoxification Chinese toad venom poison pills and lipid-based ligand content of toad poison. The results in Table 3. Table 3 Sample assay results (omitted)
Preparation method for the test product test solution, the extraction method, extraction solvent, extraction time and
solvent consumption were screened. Experimental results show that the sample with mobile phase as the solvent, ultrasonic
extraction time of 40 min can be.
HPLC Determination of 6-ling with the detoxification of the Chinese toad venom poison pills and lipid-based ligand
content of toad poison, and methods of advanced, easy to operate, accurate and can be used as six-Ling detoxification
method of quality control pills.
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