Gold Anti-quality standard of cold particles
【Abstract】 Objective To develop anti-influenza gold particles
quality standards. Methods using high performance liquid chromatography (HPLC) determination of gold particles in the anti-flu
paracetamol and chlorogenic acid. The results of the mobile phase of acetonitrile water-phosphoric acid (50:400:0.2); flow rate of 1.0 ml / min; right-acetyl amino acid detection wavelength was 244 nm, chlorogenic acid detection wavelength was 325 nm. The linear
range of acetaminophen 11.2 ~ 56.0 μg / ml, r = 0.999 1, n = 5;
chlorogenic acid in the linear range of 2.42 ~ 21.78 μg / ml, r =
0.99 8, n = 5. The average recovery of paracetamol 101.3%, RSD of 1.7%, n = 6; chlorogenic acid, the average recovery was 99.0%, RSD of
1.3%, n = 6. Conclusion The method is simple, sensitive, rapid and accurate.
Key words gold particles on anti-flu acetaminophen chlorogenic acid, high-performance liquid chromatography
AbstractObjectiveTo establish the quality control standards for
Jinfangganmao Granules.Methods The contents of Paracetamol and chlorogenic acid in Jinfangganmao Granules were determined by HPLC. ResultsMobile phase: acetonitrile-water-phosphoric acid (50:400:0.2);
flow rate: 1.0 ml / min : detection wavelength: 325 nm. The linear range of chlorogenic acid was 11.2 ~ 56.0 μg / ml, r = 0.999 1 (n =
5). The average recovery of the chlorogenic acid was 99.0%, RSD = 1.3%, n = 6 . ConclusionThe method is simple, accurate with high sensitivity and good reproducibility.
Key wordsJinfanggnmao Granules; Paracetamol; Chlorogenic Acid;
HPLC
Gold Anti-cold particles from the honeysuckle, wind, hawthorn, ginger, acetaminophen etc., has issued a antipyretic, expelling wind
and cold-dispelling function. For exogenous cold, aversion to cold sweat, fever, headache embolism. One acetaminophen, honeysuckle for Fang Jun drug, acetaminophen has antipyretic effect; honeysuckle with a heat-clearing and detoxifying, the role of wind-heat evacuation,
including chlorogenic acid, iso-chlorogenic acid and other
ingredients. In this study, pairs of agents against acetaminophen, honeysuckle contains chlorogenic acid content was studied.
1 Equipment
Gold Anti-cold particles, Lot:
020401,020402,020403,020501,020502,020503,020601,020602,020603,020604 Yellowstone by 39 pharmaceutical available; 020328,020329,020330 provided by the Hebei Pharmaceutical Hongbao.
Beckman 338 high-performance liquid chromatography, Zhejiang
University, upper chromatography workstation, Kromasil C18 (250 mm ×
4.6 mm, 5 μm) column.
Acetaminophen, chlorogenic acid reference substance of Pharmaceutical and Biological Products are offered, batch 0018-
9206,0753-200111 respectively.
2 Methods and Results
2.1 Preparation of reference substance solution
2.1.1 Paracetamol Preparation of reference substance solution precision that taking acetaminophen 14 mg, placed in 50 ml Liang Ping, add ethanol dissolved and diluted to the scale, shake.
Precision drawing 5 ml, placed in 50 ml Liang Ping, add the water was diluted to scale, shake, that was (per ml acetaminophen 28 μg).
Of chlorogenic acid reference substance solution 2.1.2 Preparation of precision that chlorogenic acid reference substance to take 10 mg, placed in 50 ml Liang Ping, add ethanol dissolved and diluted to the scale, shake. Precise amount of take 5 ml, placed in 100 ml Liang Ping, add the water was diluted to scale, shake, that was (per ml of chlorogenic acid, 10 μg).
2.2 Chromatographic conditions and determination of the wavelength selection
2.2.1 Determination of wavelength selection to take paracetamol
reference substance solution and the solution of chlorogenic acid reference substance, respectively, Shimadzu UV-2100 spectrophotometer
in the wavelength range 200-360 nm spectral scan results acetyl p-
aminophenol at 244 nm wavelength of maximum absorption of chlorogenic acid at 325 nm wavelength of maximum absorption. Because in the 244
nm and 325 nm at high sensitivity, can reduce the sample volume, reduce pollution, column, so this experiment choose 244 nm and 325 nm wavelengths were determined as the determination of paracetamol and chlorogenic acid. Wavelength conversion experiments have been used
method of injection in a case of simultaneous determination of paracetamol and chlorogenic acid, two ingredients, there are good experimental results, but considering the conditions in the apparatus without some manufacturers use.
2.2.2 The chromatographic conditions were a mobile phase of acetonitrile
Water-phosphoric acid (50:400:0.2); flow rate of 1.0 ml / min; column temperature was room temperature; paracetamol detection wavelength was 244 nm, chlorogenic acid detection wavelength was 325
nm; AUFS 0.05, injection volume 10 μl. Theoretical plate number of
acetaminophen according to the calculation, not less than 3000.
2.3 Linear Experiment
2.3.1 Paracetamol
To take paracetamol reference substance solution (280 μg / ml)
2,4,6,8,10 ml constant volume of water were added to 50 ml, each sample 10 μl, measured peak area values, the respective peak area values and The content of the respective linear regression, was the regression equation: Y = 3.575 9 × 109X-2 647.2, r = 0.999 1, n = 5.
The results show that paracetamol at 11.2 ~ 56.0 μg / ml within the
framework of a linear relationship was good. Table 1. Table 1 Standard curve of paracetamol experimental results (a) reposted elsewhere in the paper for free download http://
2.3.2 chlorogenic acid
Obtained solution of chlorogenic acid reference substance (242 μg / ml) 1,3,5,7,9 ml constant volume of water were added to 100 ml, each sample 10 μl, measured peak area values, the value of their
respective peak area with the respective The content of linear regression, was the regression equation: Y = 3.075 07 × 109X-167.37,
r = 0.999 8, n = 5. The results show that chlorogenic acid in the 2.42 ~ 21.78 μg / ml within the framework of a linear relationship
was good. Table 2. Table 2 of chlorogenic acid standard curve of experimental results (omitted)
2.4 Blank experiments
Take does not contain acetaminophen, blank samples, and research fine, fine, said appropriate amount (about the average filling level
of 1 / 20), set 50 ml Liang Ping, add ethanol 40 ml, ultrasonic treatment 10 min, Remove, place to room temperature, diluted with anhydrous ethanol to the scale, shake, filter, precision continued to take the amount of filtrate 5 ml water was diluted to 50 ml, shake,
as a blank sample solution 1. 10 μl injection determination of blank
sample results of chromatography, in with the paracetamol peak at the same time, no chromatographic peaks, that is, a blank sample without interference.
Get free samples of chlorogenic acid in the blank, and research fine, fine, said appropriate amount (about the average filling level of 1 / 20), set 25 ml Liang Ping, add ethanol 20 ml, ultrasonic treatment 10 min, removed , place to room temperature, diluted with
anhydrous ethanol to the scale, shake, filter, precision continued to take the amount of filtrate 5 ml water was diluted to 10 ml, shake, as the blank sample solution 2. 10 μl injection determination of
blank sample results of chromatography, in and chlorogenic acid peak
at the same time, no chromatographic peaks, that is, a blank sample 2 without interference.
2.5 Experiment and stability of the experimental precision obtained for the test product solution, at intervals of 1 h into the
sample a second consecutive sample six times and the results of the peak area of acetaminophen average of 100 085.6, RSD 1.0%, chlorogenic acid The average peak area of 37 808.7, RSD is 1.40%. Show that the tested materials was stable solution at 5 h, and good
precision. The results in Table 3. Table 3 Precision and stability of the experimental results (omitted)
2.6 to reproduce the experiment taken for the test batch of 20,020,401 of the goods, according to assay method of determination of five times the average levels of acetaminophen (labeled amount) was 100.3%, RSD of 1.2%, n = 5; an average of chlorogenic acid
content of 10.6 mg, RSD is 1.4%, n = 5. The results in Table 4. Table 4 reproduce the experiment results (omitted)
2.7 The average recovery obtained experimental levels have been measured for the test product 0.75 g (batch of 020,401, the average filling level of 15.05 g, paracetamol content was 0.018 59 g / g, chlorogenic acid content of 0.730 mg / g) and precision that fixed,
precision reference substance solution by adding appropriate amount (equivalent to content of the sample were 80%, 100%, 120%), according to assay method plus ethanol dissolved and measured in accordance with law. Results of acetaminophen average recovery of 101.3%, RSD of
1.7%, n = 6; chlorogenic acid, the average recovery was 99.0%, RSD of 1.3%, n = 6. The results in table 5. Table 5 Canadian sample recovery results (omitted)
2.8 Determination of results and the content of the sample the limits of golden particles 13 approved anti-influenza, according to
assay method of determination according to the law. Results (Table 6). 13 batches of samples of paracetamol content of its labeled amount of 90.0% ~ 110.0% of the range of chlorogenic acid content of
6 mg or more in the bag. However, considering the more complex varieties of honeysuckle, North and South are different sources of raw materials each enterprise, chlorogenic acid content per bag is tentatively scheduled for not less than 7.0 mg, paracetamol content
is tentatively scheduled for the labeled amount of 90.0% ~ 110.0% . Table 6 Determination of Sample Results (abbreviated)
3 Discussion
Of chlorogenic acid reference substance solution obtained on Shimadzu UV-2100 spectrophotometer in the wavelength range 200 ~ 360
nm within the spectral scan, the results of chlorogenic acid at 325 nm wavelength of maximum absorption at 325 nm at its high sensitivity, can reduce the sample volume, reduce pollution, column, so choose this experiment measured 325 nm wavelength as the
determination of chlorogenic acid.
"Chinese Pharmacopoeia" [1] 2000 edition of the Ministry of honeysuckle ? was determined by the content of acetonitrile 0.4%
phosphoric acid (40:400) as the mobile phase [2], by the measured pH
value of less than 2, in the column tolerance limit, through improved its pH value of around 3, and to better protect the column, and can achieve high column efficiency.
The experimental method has a specific, accurate, rapid and other characteristics, can be used to prevent colds gold particles
quality control.
【References】
[1] State Pharmacopoeia Commission. Chinese Pharmacopoeia, ? Department of [S]. Beijing: Chemical Industry Press, 2000:177,206.
[2] Ministry of Health, Drug Standards WS3-B-3717-98, Z19-231. Reposted elsewhere in the paper for free download http://