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Abstract A capillary electrophoresis method was developed for the first time and optimized for the determination of paracetamol, pseudoephedrine, dextromethorphan, chlorpheniramine, 4-aminophenol and ephedrine in tablet formulation. Optimum electrophoretic conditions were achieved by using a background electrolyte of 75 mmol L-1 sodium borate buffer at pH 8.0, a capillary temperature of 30°C, a separation voltage of 30 kV and a pressure injection of the sample at 50 mbar for 10 s. Calibration graphs showed a good linearity with a coefficient of determination (R2) of at least 0.999 for all compounds. Intraday and interday precision (expressed as relative standard deviation (RSD) %) were lower than 1.39% for capillary electrophoresis method. The developed method was demonstrated to be simple and rapid for the determination of paracetamol, pseudoephedrine, dextromethorphan, chlorpheniramine, 4-aminophenol and ephedrine in tablet formulation providing recoveries in the range between 99.62 and 100.57% for all analytes.
Subject(s)
Chlorpheniramine/antagonists & inhibitors , Electrophoresis, Capillary/methods , Dextromethorphan/antagonists & inhibitors , Ephedrine/antagonists & inhibitors , Pseudoephedrine/antagonists & inhibitors , Aminophenols/antagonists & inhibitors , Acetaminophen/agonists , Buffers , Diagnosis , MethodsABSTRACT
OBJECTIVE： To establish the method for simultaneous determination of ephedrine hydrochloride， pseudoephedrine hydrochloride， methamphetamine hydrochloride and paeoniflorin in Xiaoqinglong granule. METHODS： Micellar capillary electrophoresis （MCE） method was adopted. The optimum conditions for the separation were as follows as a fused silica capillary column as the separation channel， the buffer solution composed of 10 mmol/L borax-10 mmol/L SDS （95 ∶ 5， pH 10.5）， detection wavelength of 195 nm， separation voltage of 20 kV， capillary column temperature of 15 ℃，the sampling at a pressure for 0.5 psi×5 s. Two batches of Xiaoqinglong granules were collected from 2 manufacturers to determine the contents of ephedrine hydrochloride， pseudoephedrine hydrochloride， methamphetamine hydrochloride and paeoniflorin. The results of content determination were compared with the results determined by HPLC method stated in Chinese Pharmacopeia of 2015 edition. RESULTS： The linear range of ephedrine hydrochloride， pseudoephedrine hydrochloride， methamphetamine hydrochloride and paeoniflorin were 10-160， 10-160， 1-100， 10-500 μg/mL （r＝0.997 9-0.999 8）， respectively. RSDs of precision， reproducibility and stability tests were all ≤2.74％ （n＝5-6）. The average recoveries were 101.55％， 101.62％， 100.15％， 101.85％ （RSD≤3.94％， n＝6）， respectively. The contents of 4 components determined by micellar capillary electrophoresis were in accordance with the results of HPLC method. CONCLUSIONS： The established MCE method is simple， quick and sensitive， and can be used for simultaneous determination of 4 components mentioned above in Xiaoqinglong granule.
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The herbal formula, DF-02, consisting of Ephedra intermedia and Rheum palmatum are used for the treatment of the metabolic diseases such as obesity and liver fibrosis in Korean local clinics. We aimed to develop the simultaneous analytical conditions for four standards, (+)-pseudoephedrine (PSEP) and (−)-ephedrine (EP) for E. intermedia, and aloe-emodin (AE) and chrysophanol (CP) for R. palmatum using HPLC-UV techniques. The validated conditions yielded the high precision (relative standard deviation (RSD) 0.9994). As a result, four standards of DF-02 were simultaneously determined under the developed method, which will be utilized for the quality control or evaluation of DF-02 and many herbal preparations containing E. intermedia and R. palmatum.
Subject(s)
Calibration , Chromatography, High Pressure Liquid , Ephedra , Liver Cirrhosis , Metabolic Diseases , Methods , Obesity , Plant Preparations , Quality Control , RheumABSTRACT
Objective To establish a method for detecting the chemical compositions of “decocted first and defoamed” of Ephedra Herba by UPLC-DAD-TOF/MS coupled with HPLC-UV, so as to clarify the difference of chemical constituents among them. Methods The analysis was performed on an ACQUITY UPLC® BEH C18 column (50 mm × 2.1 mm, 1.7 μm ) by UPLC-DAD-TOF/MS with gradient elution. The mobile phase consists of methanol and 0.1% formic acid-water at a flow rate of 0.3 mL/min. The column temperature was 40 ℃. The information of compounds was acquired on positive and negative mode. Similarly, HPLC-UV was applied for measuring the content of alkaloids respectively. The C18 column was used, the mobile phase was acetonitrile-0.1% phosphoric acid (containing 0.05% triethylamine) (99 : 1) at the flow rate of 1 mL/min, the detective wavelength was set up at 210 nm, and the column temperature was 30 ℃. Results There were less content in the upper foam, and the chemical components in the lower liquid and the whole liquid were basically same. Five alkaloids and one carboxylic acid (4-hydroxy-7-methoxyl-2-quinoline carboxylic acid) was identified from all kinds of liquids. However, the content of alkaloids in the upper foam was very low, and the content of three alkaloids in the whole solution was slightly higher than that in the lower liquid. Conclusion The defoamed method may not be related to the chemical compositions of alkaloids, but it still needs further research and verification.
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Objective To optimize extraction process of Qinhao Nasal Drops by multi-index comprehensive evaluation Method. Methods With L9(34) orthogonal design, the content of rupestonic acid, chlorogenic acid, pseudoephedrine hydrochloride, total flavonoids and extract yield were set as indexes, and extraction technology of Qinhao Nasal Drops was optimized.Results Optimum extraction technology was:12 times amount of 60% ethanol, extracted three times. Conclusion The optimized extraction technology is simple, practical, and adapt to the production needs, which can be used as the basis for reasonable development of the preparation.
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AIM To establish an HPLC method for the simultaneous content determination of four constituents in Kesuting Capsules (a fast cough suppressant,containing Ephedrae Herba,Papaveris Pericarpium,Platycodonis Radix,etc.).METHODS The analysis of trichloromethane-strong ammonia extract of Kesuting Capsules was performed on a 35 ℃ thermostatic Welch Ultimate(◎) XB-C18 column (4.6 mm ×250 mm,5 μm),with the mobile phase comprising of acetonitrile-0.01 mol/L potassium dihydrogen phosphate buffer flowing at 1.0 mL/min in an isocratic elution manner,and the detection wavelength was set at 210 nm.RESULTS Morphine,ephedrine hydrochloride,pseudoephedrine hydrochloride and codeine phosphate showed good linear relationships within the ranges of 8.054-67.12 μg/mL (r =0.999 5),22.31-185.9 μg/mL (r =0.999 9),21.26-177.2 μg/mL (r =0.999 7) and 1.212-10.09 μg/mL (r =0.999 7),whose average recoveries (n =9) were 100.9％ (RSD =2.0％),101.4％ (RSD =3.6％),105.3％ (RSD =1.2％) and 106.2％ (RSD =1.2％),respectively.CONCLUSION This simple method can be used for the rapid quality control of Kesuting Capsules.
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DF formula is comprised of three traditional herbs, Ephedra intermedia, Rheum palmatum and Lithospermum erythrorhizon, and locally used for treating of the metabolic diseases, such as obesity and diabetes in Korea. We tried to optimize the extraction conditions of two major components, (−)-ephedrine and (+)-pseudoephedrine, in DF formula using response surface methodology with Box-Behnken design (BBD). The experimental conditions with 70% for EtOH concentrations, 4.8 hour for extraction hours and 8.7 times for the solvent to material ratio were suggested for the optimized extraction of DF formula with the highest amounts of (−)-ephedrine and (+)-pseudoephedrine in the designed model.
Subject(s)
Chromatography, High Pressure Liquid , Ephedra , Korea , Lithospermum , Metabolic Diseases , Obesity , RheumABSTRACT
OBJECTIVE:To study the new formula of effective components in TCM for anti-allergic rhinitis (AR),and pro-vide reference for developing TCM preparations for anti-AR. METHODS:Using pseudoephedrine hydrochloride (0-13.5 mg/kg), total alkaloid extracts of Aconitum carmichaelii (0-21.18 mg/kg),volatile oil of asari radix (0-0.0092 mL/kg) in Mahuang Fuzi Xixin decoction as formula objects,uniform design method was used for drug grouping,and multiple regression analysis was con-ducted for the behavioral scores before and after administration,contents of histamine and immunoglobulin E (IgE) in serum of AR guinea pigs to obtain the best formula. Using Xinqin granule,Loratadine tablet,Mahuang Fuzi Xixin decoction respectively as positive control,efficacy of the best formula was verified from aspects of behavioral scores before and after administration,con-tents of histamine and IgE of AR guinea pigs. And the safety of the best formula was preliminarily observed through acute toxicity test in mice. RESULTS:The best formula was as follow as pseudoephedrine hydrochloride 11.25 mg/kg,total alkaloid extracts of A. carmichaelii 21.18 mg/kg,volatile oil of asari radix 0.0045 mL/kg. Compared with each positive drug group,there were no sig-nificant differences in behavioral scores before and after administration in the best formula group(P>0.05). While compared with Xinqin granule group and Mahuang Fuzi Xixin decoction group,histamine content in serum in the best formula group was signifi-cantly reduced (P<0.05);compared with Xinqin granule and Loratadine tablet group,IgE content in serum in the best formula group was significant decreased (P<0.05). Median lethal dose of the best formula was 1822.04 mg/kg. CONCLUSIONS:The screened best formula shows better effect than Xinqin granule and Mahuang Fuzi Xixin decoction in terms of reducing histamine content in serum,better than Loratadine tablet and Xinqin granule in terms of reducing IgE content in serum,with good safety, which indicates the feasibility of TCM effective component formula to a certain degree.
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Objective: To explore the optimal separation and purification of extract in Sanao Sustained-release Tablets. Methods: Taking the adsorption ratio and desorption ratio of ephedrine hydrochloride, pseudoephedrine hydrochloride, amygdalin, and glycyrrhizinate as evaluation indexes to optimize the purification process of Sanao Sustained-release Tablets by multi index comprehensive score. Results: Macroporous resin HPD 300 had the best adsorption and desorption properties. In the course of adsorption, the optimum concentration of the sample liquid was 1.67 g crude drugs of per milliliter, the resin column size ratio was 1: 7, the concentration of sample solution was 0.6 g/mL crude drug, the sample flow rate was 4.0 BV/h. In the course of elution, 2 BV deionized water was used and the resin column chromatography was eluted with 5 BV of 70% EtOH by flow rate of 3 BV/h. Conclusion: Macroporous resin HPD 300 is suitable to separate and purify the extract from Sanao Sustained-release Tablets.
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Objective To establish a capillary electrophoresis method to separate ephedrine and psedudoephedrine. Methods RM-β-CD and HP-β-CD were set as additives. A capillary electrophoresis method was set up. The effects of types and concentrations of additives, the concentrations and pH values of buffered solution, running voltage and organic solvent on the separation of ephedrine and psedudoephedrine were investigated.Results Ephedrine and pseudoephedrine could be successfully separated by using either RM-β-CD or HP-β-CD as additives. When RM-β-CD was used as additive, the best separation conditions were as follows: separation voltage 10 kV, 25 mmol/L Tris-H3PO4 (pH 2.42), 20 mg/mL of RM-β-CD. Under the conditions, the resolution of ephedrine and pseudoephedrine was 1.56 and they were separated successfully within 13 min. When HP-β-CD was used as additive, the best separation conditions were as follows: separation voltage 10 kV, 25 mmol/L Tris-H3PO4 (pH 3.00), 50 mg/mL of HP-β-CD. Under the conditions, the resolution of ephedrine and pseudoephedrine was 2.73 and they were separated successfully within 15 min.ConclusionThis method is reliable, rapid and repeatable. It can be used as separation determination method for ephedrine and pseudoephedrine.
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Ischemic colitis is the consequence of a sudden reduction in colon blood supply, which in turn results in ischemic injury. The splenic flexure and rectosigmoid junction are the areas most often affected. Ischemic colitis occurs with greater frequency in the elderly and is caused by various medications and procedures. Pseudoephedrine acts as a vasoconstrictor directly affecting adrenal receptors of nasal mucous membrane. Pseudoephedrine occasionally causes vascular insufficiency due to intense vasoconstriction, even at standard doses. Ischemic colitis associated with pseudoephedrine has been reported in other countries,, but it has never been reported in Korea. In this paper, we describe 3 cases of ischemic colitis that occurred after taking pseudoephedrine for nasal congestion.
Subject(s)
Aged , Humans , Colitis, Ischemic , Colon , Colon, Transverse , Estrogens, Conjugated (USP) , Gastrointestinal Hemorrhage , Korea , Mucous Membrane , Pseudoephedrine , VasoconstrictionABSTRACT
Objective: To clarify the influence of the different combinations (consumption, fillers) of Improved Peach Gum to the balance release of complex components. Methods: Use Chuanping Prescription as model drug, Improved Peach Gum as sustained release materials, the release test companied with HPLC was applied to determine the accumulated release rate of the index components (ephedrine, pseudoephedrine, scopolamine) in Chuanping Sustained-release Tablets, calculate the cumulative release curve slope K value, and to evaluate the balance release of the different components. Results: The study on different combinations, when the filler is starch, starch/dextrin, and starch/MCC, the index component cumulative release curves were close to slope K value and can achieve the balance release; match with dextrin and MCC, the slope K values are different and can not achieve the balance release. With increasing the amount of Improved Peach Gum, release time prolonged, cumulative release slope K values of index components are basically same and can achieve balance release. Conclusion: Different fillers match with Improved Peach Gum can affect the balance release of complex components of Chinese materia medica; Different amount of Improved Peach Gum will affect the drug release time, but not affect on balance release.
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Objective To establish an HPLC method for determination of ephedrine hydrochloride and pseudoephedrine hydrochloride in Maxing oral solution .Methods Phenomenex Hydro-RP (250 mm × 4 .6 mm ,4 μm) was adopted .Acetonit-nile (A) and 0 .1% phosphonic acid solution (0 .1% triethanolamine solution)(B) was used as gradient mobile phase(0-20 min , 3% →10% A)at flow rate was 1 .0 ml/min and the program of UV gradient absorbance detection was 210 nm .The sample vol-ume was 20 μl .Results A good linearity was obtained over the concentration range of 0 .99-39 .6 μg/ml for ephedrine hydro-chloride (r=0 .999 9) and 1 .09-43 .6 μg/ml for pseudoephedrine hydrochloride (r=0 .999 9) .The average recovery of ephed-rine hydrochloride was 101 .5% with RSD of 1 .77% (n=6) ,and the average recovery of pseudoephedrine hydrochloride was 100 .8% with RSD of 1 .96% (n=6) .Conclusion This method was simple ,accurate and quick ,which could be used for deter-mination and quality control of Maxing oral solution with good selectivity and repeatability .
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Aims: UV Spectrophotometric Method for the Simultaneous Determination of Desloratidine and Pseudoephedrine HCl in combined Dosage form. Study Design: A simple, rapid and specific UV spectroscopic method with good sensitivity was developed and validated for the simultaneous determination of Desloratidine and Pseudoephedrine HCl in bulk and pharmaceutical dosage form. Place and Duration of Study: Department of pharmaceutical Analysis & Quality Assurance, School of Pharmacy, Anurag Group of Institutions, Venkatapur, R.R Dist, Andhra Pradesh, India during February 2013 and April 2013. Methodology: Vierodt’s (Simultaneous equation) method was performed for Estimation of Desloratidine and Pseudoephedrine HCl in Pharmaceutical dosage form. Results: In Ethanol the max of Desloratidine and Pseudoephedrine HCl was fixed as 240 and 258 nm respectively using a Shimadzu UV-Visible spectrophotometer. In this proposed method both drugs obeyed linearity within the concentration range of 5-30 g/ml and 80-800 g/ml for Desloratidine and Pseudoephedrine HCl respectively. The low RSD values indicate good precision and high recovery values indicate accuracy of the proposed method. The proposed method has been applied to the determination of drugs in commercial formulations. Assay results were in good agreement with label claim. The method was validated as per ICH guidliness. Conclusion: The developed method was simple, accurate, precise, specific, sensitive and reproducible which can be efficiently and easily applied to pharmaceutical dosage forms.
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Objective: To observe the effect of Cinnamomi Ramulus on the distribution kinetics of ephedrine (E) and pseudoephedrine (PE) from Ephedrae Herba in brain tissues of mice. Methods: Mice were ig adminstered by Cinnamomi Ramulus and codecoction of Cinnamomi Ramulus combined with Ephedrae Herba. Brain tissues of mice were collected at different time after drug administration. The variation of E and PE with time was determined by GC-MS method. The non compartmental kinetic was fitted and the parameters were calculated by Kinetica 5.0.11 software, so as to evaluate the effect of Cinnamomi Ramulus on the distribution kinetics of E and PE from Ephedrae Herba in brain tissues of mice. Results: Compared with the Ephedrae Herba group, in the group with the codecoction of Cinnamomi Ramulus combined with Ephedrae Herba, the tmax of E and PE distributed in the brain tissues of mice was delayed, the AUC0-∞ of E and PE in the brain tissues of mice under the drug concentration curve was smaller and the MRT0-∞ of E was reduced. Conclusion: Cinnamomi Ramulus combined with Ephedrae Herba has the propertis of delaying the distribution process of E and PE, reducing the cumulative distribution volume, and accelerating the elimination of E and PE in the brain tissues of mice. Above all, Cinnamomi Ramulus can relieve the neurotoxicity of Ephedrae Herba, and there is the combination function of mutual restraint and mutual supression between the two drugs.
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Objective To establish the method for determining ephedrine hydochloride and pseudoephedrine hydrochloride in Keke Tablets by HPLC. Methods The samples were analyzed by a phemomenex Synergi Polar-RP column (4.6 mm×250 mm, 4 μm), with mobile phase methanol∶0.092%phosphoric acid (0.04%triethylamine and 0.02%second butylamine)=1.5∶98.5 at flow rate of 1.0 mL/min and detection at UV wavelength of 210 nm. The column temperature was 30 ℃. Results The linear ranges of ephedrine hydrochloride and pseudoephedrine hydrochloride were 6.51×10-3-0.651 μg (r=0.999 9) and 6.27×10-3-0.627 μg (r=1), respectively. The average recoveries (n=6) of ephedrine hydrochloride and pseudoephedrine hydrochloride were 102.26%and 103.71%, with RSD of 0.34%and 0.22%, respectively. Conclusion This method is simple, accurate, reproducible, highly specific and reliable results, and has the ability to effectively control the quality of alkaloids in Keke Tablets.
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Amostras de Ephedra tweediana Fisch & C.A. Meyer, coletadas de populações nativas da Reserva Biológica do Lami José Lutzenberger (Porto Alegre, RS, Brasil), e amostras de Ephedra triandra Tul., obtidas de plantas cultivadas em Porto Alegre/RS, foram extraídas com acetona, derivatizadas com ciclohexanona e analisadas por CG/EM. Para verificação da eficiência da metodologia, além das amostras de Ephedra tweediana e E. triandra, foram analisadas cinco amostras comerciais de Ephedra, de procedências distintas, cedidas por farmácias de manipulação locais. Os resultados encontrados indicam a ausência de efedrinas em Ephedra tweediana e E. triandra e presença de efedrina e/ou pseudoefedrina nas amostras comerciais.
Samples of Ephedra tweediana, collected from native populations occurring in the Reserva Biológica do Lami José Lutzenberger (Porto Alegre, RS, Brazil), and from cultivated plants of Ephedra triandra were submitted to extraction with acetone, derivatized with cyclohexanone and analyzed by GC/MS. In order to verify the efficiency of the methodology, besides Ephedra tweediana and E. triandra, samples of five commercial Ephedra extracts were analyzed, from distinct origins, get up from local drugstores. The results showed the absence of ephedrines in Ephedra tweediana and E. triandra, and the presence of ephedrine and/or pseudoephedrine in commercial samples.
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Rhinos® SR is a fixed combination of 5 mg loratadine and 60 mg pseudoephedrine immediate release and 60 mg pseudoephedrine sustained release. The present study was aimed to assess the efficacy of Rhinos® SR on nasal airway resistance (NAR) objectively using rhinomanometer and on nasal symptoms in patients with perennial allergic rhinitis (PAR) in a tropical country. This was a randomized, double-blind, parallel group study in 59 PAR patients who visited the ENT clinic at Dr. Soetomo General Hospital, Surabaya. Outpatients of both gender, having moderate to severe PAR for a minimal of 2 years, aged 12 years or older, with a total nasal symptom score (TNSS) > 6 and a nasal congestion score > 2, received Rhinos® SR or placebo twice daily for 7 days. The primary efficacy parameter was the decrease in the NAR values (measured by rhinomanometer on Day 1) of Rhinos® SR from those of placebo. The NAR values were calculated as the area under the curve (AUC) of NAR versus time. The secondary efficacy parameters were the percentage reduction of the clinical symptoms (nasal and nonnasal) evaluated by both the patient and the physician after 1 week use of Rhinos® SR or placebo. From 59 eligible patients, all completed this 1-week trial. For NAR values, after the baseline were considered as 100%, the AUC0-10 h were not significantly different between Rhinos® SR and placebo. However, as the pseudoephedrine reached its peak concentration, i.e. 2 hrs for the immediate release and 6 hrs for the sustained release, then AUC0-2 h and AUC0-6 h of Rhinos® SR were significantly lower compared to those of placebo. Total nasal symptom score (TNSS) evaluated by the patient (sum of the last 3 mornings) for Rhinos® SR decreased 33.0% from baseline (p < 0.001), for placebo decreased 21.9% from baseline (p = 0.002), but the decrease by Rhinos® SR was not significantly different from the decrease by placebo. TNSS evaluated by the physician, nasal congestion score (NCS) and total symptom score (TSS, total nasal and nonnasal), and even the individual symptom scores, evaluated by the patient and the physician, showed similar pattern, i.e. both Rhinos® SR and placebo decreased the symptoms significantly from baseline, and the decreases by Rhinos® SR were larger than the decreases by placebo, but the decreases by Rhinos® SR and placebo were not statistically different. No adverse event was found in this study. From the present study it was concluded that in patients with moderate to severe PAR in a tropical country, Rhinos® SR was effective in relieving nasal congestion by objective measurements of NAR. Rhinos® SR twice a day for 7 days was also effective in reducing the clinical symptoms of PAR although the reductions did not reach statistical significance compared to those by placebo, and was well tolerated.
Subject(s)
Rhinitis , Pseudoephedrine , LoratadineABSTRACT
OBJECTIVE:To determine the concentration of pseudoephedrine hydrochloride in human plasma by LC/MS. METHODS:The separation of sample was performed on Zorbax Eclipse XDB C18 with diphenhydramine used as the internal standard.The mobile phase was a mixture of methanol-water(10mmol?L-1 NH4Ac plus 0.1% acetic acid)(55∶45) with a flow rate of 0.2mL?min-1.The column temperature was set at 30℃.The atmospheric pressure chemical ionization-mass spectrometry(APCI-MS) were adopted with pseudoephedrine m/z =166.1 and diphenhydramine m/z =242.3.RESULTS:The linear concentration range for pseudoephedrine was 3.2～408.96ng?mL-1(r=0.999 0) with lowest detection limit at 3.2ng?mL-1.The average recovery was 98.21% with both the intra-day RSD and the inter-day RSD at less than 13%.The stability of pseudoephedrine was stable.CONCLUSION:The method is of high sensibility and accuracy,and it can be used for blood concentration monitoring pharmacokinetic study of pseudoephedrine.
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A new spectrophotometry was described for the simultaneous analysis of pseudoephedrine sulfate-Ioratadine combination. The derivative spectrophotometry dA/d values were read at zero-crossing point. Mean recoveries were found to be more than 98% for these compound in mixture. The procedure does not require any separation step and proven to be rapid, simple and accurate for determination of the mentioned sample or corresponding multi-component mixture