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Objective To improve the quality control of Dilong Shenmai oral liquid. Methods TLC was used for the qualitative identification of Astragali Radix, Ophiopogonis Radix and Schisandrae Chinensis Fructus in Dilong Shenmai oral liquid. HPLC was used to determine the contents of schisandrin and ethylparaben in the preparation. Wondasil C18 column (250 mm×4.6 mm, 5 μm) was used with acetonitrile-water as the mobile phase at the flow rate of 1.0 ml/min for gradient elution. The detection wavelength was set at 254 nm, and column temperature was 30 ℃. Results TLC spots were clear and well-separated without negative interference. The linear ranges of schisandrin and ethylparaben were 5.81−58.06 μg/ml (r=0.999 9) and 25.29−252.94 μg/ml (r=0.999 9). The average recoveries were 99.35% (RSD=1.02%) and 99.72% (RSD=0.76%). Conclusion This method is simple, quick and accurate. It can be used for effective quality control of Dilong Shenmai oral liquid.
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Background and Objectives:Parabens are one of the chemicals used widely in preserving foods and pharmaceutical preparations. Although it was safe for many years, recently it has been proven that its action mimics estrogen in the body when it is linked to its receptors, known as estrogen receptors which are present in many systems of the body and that it may have a link with breast cancer, especially after it was found in samples of breast cancer. As known that estrogen receptors are placed in different areas in the body, including the stomach, therefore it may have a role in cancer formation and development in the stomach.The purpose of this manuscript is to investigate the presence of Methyl, Ethyland Propylparaben in stomach cancer in men and women.Methods:Samples of stomach cancer have been collected immediately after surgery in Al Assad University Hospital and after extracting parabens from samples, they have been analyzed by HPLC / MS in the science faculty at Damascus University.Results:All samples have the three types ofparabens with total mean concentration (22.5 ± 0.4 ng/g).The concentration of Methylparaben was the highest (8.2 ± 0.3 ng/g) then Propylparaben (7.4 ± 0.4 ng/g) and finally Ethylparaben (6.9 ± 0.2 ng/g).Conclusion: Because of the presence of parabens inall stomach cancer samples, so more studies must be done to research if parabens may have any effect in the formation of abnormal cells and the formation of cancer in the body systems which have estrogen receptor
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OBJECTIVE: To evaluate the bacteriostatic efficacy of diclofenac sodium eye drops and to explore the reasonable dose of benzalkonium chloride, ethylparaben and thimerosal in diclofenac sodium eye drops. METHODS: According to the method of bacteriostatis effect test in 2015 edition of Chinese Pharmacopoeia (Ch.P),and Escherichia coli, Staphylococcus aureus, Pesudomonas aeruginosa, Candida albicans and Aspergillus niger as test strains,the bacteriostatis effect of diclofenac sodium eye drops from 10 batches of the samples was determined. Also, the concentration gradient of benzalkonium chloride, ethylparaben and thimerosal in diclofenac sodium eye drops was designed to investigate the optimum bacteriostatic concentration. RESULTS: The samples from 3 manufacturers could reach level B, no sample could reach level A,and those from 7 manufacturers did not comply with the specification. When the concentration of thimerosal was 0.01 mg•mL-1 and the concentration of ethylparaben was 0.3 mg•mL-1 in diclofenac sodium eye drops, the bacteriostatic efficacy could reach level B. When the concentration of benzalkonium chloride was 0.01 mg•mL-1, the bacteriostatic efficacy could reach level A. CONCLUSION: The bacteriostatis effect of diclofenac sodium eye drops from 10 batches of the samples is not good, It is recommended that these manufacturers should optimize the type and concentration of antimicrobial agents and optimize their formulation based on both biological tests and physical-chemical tests to ensure drug safety.
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SUMMARY Solubility data of bioactive compound such as ethylparaben (EtP) are important for the scientific and community. Therefore, in present study, solubility, solution thermodynamics and solute-solvent interactions (at molecular level) of EtP in nine cosolvent mixtures (1-propanol {n-PrOH) (1) + methanol (MeOH) (2)} including pure solvent (methanol and 1-propanol) at three different temperatures, i.e. (T = 283.2 K, 298.2 K, and 313.2 K) and constant pressure (p = 0.1 MPa) were studied. Experimental solubility of EtP (expressed in mole fraction) was observed highest in n-PrOH at 313.2 K, so, mole fraction solubility of EtP (x3) increases when temperature arises and increases with n-PrOH proportion increasing. Ideal solubilities of EtP were estimated using their thermal parameters at three different temperatures. Ideal solubilities of EtP were observed similar to experimental solubilities of EtP at each temperature. With the help of ideal solubilities of EtP, activity coefficients were estimated. Based on estimated values of activity coefficients, highest interactions at molecular level were observed in rich-MeOH mixtures. Apparent thermodynamic analysis data showed endothermic and enthalpy-driven dissolution of EtP in each solvent and mixture studied. Solubility behavior was adequately correlated by means of the van't Hoff and Yalkowsky-Roseman models combined.
RESUMEN La solubilidad de compuestos bioactivos como el etilparabeno (EtP) es importante para la comunidad científica. Por lo tanto, en el presente estudio se reportan la solubilidad, termodinámica de solución e interacciones soluto-solvente (a nivel molecular) del EtP en nueve mezclas de cosolventes {1-propanol (n-PrOH) (1) + metanol (MeOH) (2)} incluyendo los solventes puros (metanol y 1-propanol) a tres temperaturas diferentes, (T = 283,2 K, 298,15 K y 313,2 K) y a presión constante ( p = 0,1 MPa). La solubilidad experimental más alta del EtP (expresadas en fracción molar) se registró en n-PrOH a 313,15 K, así, la solubilidad en fracción molar de EtP aumenta cuando la temperatura aumenta y la proporción de n-PrOH aumentan. Las solubilidades ideales de EtP se estimaron utilizando los parámetros térmicos a tres temperaturas diferentes. Las solubilidades ideales de EtPa son similares a las solubilidades experimentales de EtP a cada temperatura. A partir de las solubilidades ideales de EtP se estimaron los coeficientes de actividad y sobre la base de los valores estimados de los coeficientes de actividad, se define que las interacciones más altas a nivel molecular se registraron en mezclas ricas en MeOH. Los datos aparentes del análisis termodinámico mostraron un proceso endotérmico con conducción entálpica para el EtP cada uno de los solventes y mezclas de solventes estudiados. El comportamiento de solubilidad se correlacionó adecuadamente mediante los modelos de van't Hoff y Yalkowsky-Roseman combinados.
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OBJECTIVE: To screen out suitable antibacterial agent and reasonable dosage for timolol maleate eye drops. METHODS: According to the method of bacteriostatic effect test in Chinese Pharmacopoeia (Ch.P) 2015, the antimicrobial effectiveness of antimicrobial preservatives at different concentrations was tested to screen out the optimal agent and dosage. RESULTS: The eye drops added with ethyl hydroxybenzoate met the B-level requirements of bacteriostatic efficacy, which was the same as the sample without antibacterial agent, so ethyl hydroxybenzoate was not suitable as the antimicrobial preservative. The growth of five kinds of test microorganisms was inhibited effectively by 0.03 mg·mL-1 benzalkonium bromide. The timolol maleate eye drops with 0.03 mg·mL-1 benzalkonium bromide met the requirement of the quality standard. CONCLUSION: Benzalkonium bromide can be used as the antimicrobial preservative for timolol maleate eye drops.
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Objective: To investigate the content of ethylparaben in potassium chloride solution.Methods: According to the guidance for antibacterial effect test stated in Chinese Pharmacopoeia(the 4th volume of 2015 edition), 5 standard bacterial strains including Staphylococcus aureus,Escherichia coli,Pseudomonas aeruginosa,Candida albicans and Aspergillus niger were used as the challenging strains.Using the logarithm decrease of bacteria number as the index, the antimicrobial effectiveness of ethylparaben at different concentrations was studied to screen out the optimal concentration in the solution.Results: The growth of the 5 standard bacterial strains was inhibited effectively by potassium chloride solution containing 0.05% ethylparaben, which was also the minimum effective concentration.Conclusion: 0.05% Ethylparaben is suitable as the bacteriostatic agent for potassium chloride solution.
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Objective: To establish an ion chromatography (IC) method to determine the content of chloride ion and sulfate ion in ethylparaben, and evaluate the quality status of chloride ion and sulfate ion in ethylparaben at different levels.Methods: Ion chromatograph was used.The column was Dionex IonPac AS 18 (250 mm ×4 mm,5 μm) using potassium hydroxide as the mobile phase with gradient elution, the flow rate was 1.0 ml·min-1 , the injection volume was 25 μl, and the quantitative method was standard curve.Results: The method showed good linear relationship within the range of 0.02-4.00 μg·ml-1 for chloride ion (r=0.999 9) and 0.10-10.00μg·ml-1 for sulfate ion (r=0.999 5).The average recovery was 90.12% (RSD=3.4%) and 85.54% (RSD=6.2%) for chloride ion and sulfate ion, respectively (n =9).The content range of chloride ion and sulfate ion was 0.000 3%-0.015 7% and 0.000 9%-0.024 4% in 63 batches of samples, respectively.Conclusion: The established method is simple, fast and accurate, which can be used to determine the contents of chloride ion and sulfate ion in ethylparaben and is helpful to its quality control.
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OBJECTIVE:To establish a method for simultaneous determination of residual methylparaben,ethylparaben,nipa-sol and benzalkonium chloride in marketed eye drops. METHODS:HPLC method was adopted. The determination was performed on Hypersil GOLD C18 column with mobile phase consisted of 0.005 mol/L ammonium acetate(10 mL triehtylamine in 1 L solu-tion,pH adjusted to 5.0±0.5 with glacial acetic acid)-acetonitrile(45:55,V/V)at the flow rate of 1.0 mL/min. The detection wave-length was 262 nm(methylparaben,ethylparaben,nipasol)and 214 nm(benzalkonium chloride),respectively. The column tem-perature was 30 ℃ and sample size was 20 μL. RESULTS:The linear range were 1.2350-15.4380 μg/mL for methylparaben(r=0.9999),1.3170-16.3836 μ g/mL for ethylparaben (r=0.9997),1.2072-15.0894 μ g/mL for nipasol (r=0.9996) and 17.776-222.0 μg/mL for benzalkonium chloride(r=0.9999),respectively. Limits of quantitation were 2.0,2.0,2.0,1.11 μg,re-spectively;limits of determination were 0.375,0.375,0.375,0.333 μg,respectively. RSDs of precision,stability and reproducibili-ty tests were all lower than 2.0%. The average recoveries were 98.14%-102.48%(RSD=1.6%,n=9),98.79%-102.42%(RSD=1.3%,n=9),98.19%-102.49%(RSD=1.5%,n=9)and 98.76%-100.53%(RSD=0.6%,n=9),respectively. CONCLUSIONS:The method is accurate,reproducible,simple and suitable for the determination of residual methylparaben,ethylparaben,nipasol and benzalkonium chloride in marketed eye drops.
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Background It is imperative for the microbial monitor after opening the bottle of eyedrops in order to ensure the safety during use of ophthalmic solutions with multi-dose packaging.Objective This study was to research the microbiological properties and sterile duration of methylcellulose (MC) eye drops in three common environmental conditions,including room temperature condition of community,refrigeration condition of community and room temperature condition of hospital.Methods MC eye drops were assigned to the community room temperature group,community refrigeration group and hospital room temperature group,and 200 bottles of MC eye drops with or without ethylparaben were collected in each group,including sealed or unsealed drugs at average.The containers of all the eye drops were opened and the opening times were record.The drugs was admistered 1 drop for 3 times per day,with the opening period for 5-10 seconds.Then the drugs were preserved in different environments based on grouping.Microbial isolation and purification were performed by the same lab technician at 8:00 from 1 through 10 days after opening of drugs with automatic microbial analyzer.Results In the unsealed MC eye drops without ethylparaben,the bacterial positive rates were about 30％ in the community room temperature group,community refrigeration group and hospital room temperature group,but no microbial colony was seen in the sealed eye drops.Ten days after opening of containers,the bacterial cultured rates were 30％,32％ and 36％ in the eye drops without ethylparaben in the community room temperature group,community refrigeration group and hospital room temperature group,and those in the eye drops with ethylparaben were 15％,19％ and 23％,respectively,showing significant differences between the eye drops with and without ethylparaben (x2 =6.452,4.448,4.063,all at P＜0.05).The 95％ confidence interval (CI) of difference values of intergroup bacterial rates were-0.166-0.126,-0.110-0.190 and-0.088-0.208 between the community room temperature group and the community refrigeration group,between the hospital room temperature group and the community refrigeration group,between the hospital room temperature group and the community room temperature group respectively in the unsealed eye drops without ethylparaben,and those in the unsealed eye drops with ethylparaben were-0.159-0.079,-0.089-0.169 and-0.043-0.203 respectively,indicating insignificant differences among the groups.Cultured bacteria were identified as Micrococcus luteus,Acinetobacter lwoffii,Bacillus subtilis,Acinetobacter radioresistens,Myroides and Staptococcus xylosus.Conclusions Ethylparaben can reduce the contamination rate of microorganisms after opening of MC eye drops.Three environmental conditions do not play an influence on microbial contamination of MC eye drops after opening.The bacteria of contaminated eye drops appear to be common microorganisms in atmosphere and soil,rather than eye common pathogens.
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Objective: To study whether domestic chloramphenicol eye drops with different ethylparabenin content meet the re-quirements in Chinese Pharmacopoeia. Methods:Antimicrobial effect test was used to examine the antimicrobial effect of the different eye drops. Results:The antimicrobial effect of the eye drops was in compliance with the requirements in the pharmacopoeia. Conclu-sion:The ethylparabenin concentration in the eye drops is higher than necessary. Boric acid and borax not only can adjust pH, but also show antimicrobial effect.
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OBJECTIVE: To establish a RP-HPLC method for the determination of preservative ethylparaben content in hospital preparation.METHODS: The determination was carried out on Spherisorb C18 column and the mobile phase consisted of acetonitrile-water(50∶50,V/V) at a flow rate of 1 mL?min-1.The column temperature was set at 35 ℃;the detection wavelength was set at 254 nm and the sample size was 20 ?L.RESULTS: The linear range of ethylparaben was 1.812 5～18.125 0 ?g?mL-1(r=0.999 9) with an average recovery rate of 99.92%.The intra-day RSD was less than 2.10% and inter-day RSD was less than 4.89%.CONCLUSION: The method is simple,rapid and accurate,and applicable for the determination of ethylparaben content in hospital preparation.
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OBJECTIVE:Dual-wavelength spectrophotometry was developed for the determination of ciprofloxacin lactate in its eye drops.METHODS:Detection was performed at wavelength 237nm and 279nm with 0.1mol/L HCl as diluent.RESU_LTS:The assay was linear for ciprofloxacin lactate in the concentration range of 3～9?g/ml,r=0.9 998;The mean recovery was 101.6%,RSD was 2.16%.CONCLUSION:This method is simple,quick,accurate and suitable for the determination of ciprofloxacin lactate in its eye drops.