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OBJECTIVE：To optimi ze and improve the quality standard for Keqing capsules. METHODS ：According to general rule 0502 method stated in 2015 edition of Chinese Pharmacopeia （part Ⅳ），TLC method was used to identify Reineckia carnea and Morus alba in Keqing capsules [the developing solvents were dichloromethane-ethyl acetate-formic acid （10 ∶ 4 ∶ 0.2，V/V/V） and ethyl acetate-carbinol-ammonia （12 ∶ 2 ∶ 1，V/V/V），respectively]. The contents of morphine and codeine phosphate in Keqing capsules were determined by HPLC. The determination was performed on XBridge C 18 column with mobile phase consisted of acetonitrile-0.01 mol/L potassium dihydrogen phosphate aqueous solution （pH value adjusted to 2.7 with 5％ phosphoric acid solution）（5 ∶ 95，V/V）at the flow rate of 1.0 mL/min. The detection wavelength was set at 210 nm，and the column temperature was 35 ℃. The sample size was 10 µL. RESULTS ：In TLC of R. carnea and M. alba in samples ，same color spots were shown in the correspon ding positions of reference substance chromatogram without interference from negative control. The linear range of morphine and codeine phosphate were batches of Keqing capsules were 0.97-1.37，0.16-0.37 mg/g，respectively. CONCLUSIONS ：TLC identification method for R. carnea and M. alba ，as well as HPLC content determination method for morphine and codeine phosphate in Keqing capsules are established；the method is simple ，accurate and reliable with strong specificity ，which improves the quality standard of Keqing capsules.
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Objective: To improve the quality standard for Qiangli Pipa distillate formula. Methods: The chemical reactions for i-dentification in the old standard were deleted. TLC methods were established to identify Papaveris pericarpium, Eriobotryae folium and Platycodonis radix. The contents of morphine and codeine phosphate from Papaveris pericarpium were determined by HPLC. The chro-matographic conditions for morphine content determination were as follows: an Inertsil ODS-3 chromatographic column (250 mm × 4. 6 mm, 5 μ m ) was used, the mobile phase was acetonitrile-the mixture of 0. 01 mol·L-1sodium heptane sulfonate and 0. 02 mol ·L-1potassium dihydrogen phosphate with equal amount (10% phosphoric acid was used to adjust pH to 2. 8) ( 13: 87 ), the detec-tion wavelength was 220 nm ,the column temperature was 30 ℃, and the flow rate was 1. 0 ml·min-1. The chromatographic condi-tions for codeine phosphate content determination were as follows : an Inertsil ODS-3 chromatographic column (250 mm×4. 6 mm, 5 μ m ) was used, the mobile phase was acetonitrile-the mixture of 0. 01 mol·L-1sodium heptane sulfonate and 0. 02 mol·L-1s potas-sium dihydrogen phosphate with equal amount (10% phosphoric acid was used to adjust pH to 2. 8) ( 15: 85 ), the detection wave-length was 220 nm, the column temperature was 30 ℃, and the flow rate was 1. 0 ml·min-1. Results: TLC had obvious characteris-tics with clear and well-separated spots. Morphine showed a good linear relationship within the range of 3. 14-62. 8 μg·ml-1( r=1. 000 0) with the average recovery of 96. 69% (RSD=2. 41% , n=9). Codeine phosphate showed a good linear relationship within the range of 3. 52-87. 94 μg·ml-1(r=1. 000 0) with the average recovery of 95. 68% (RSD=2. 64% , n=9). Conclusion: The quality standard for Qiangli Pipa distillate formula is improved. The methods are easy-operated and accurate with good specificity, which are suitable for the quality control of Qiangli Pipa distillate formula.
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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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Objective:To establish a method to determine the content of morphine and codeine phosphate in compound liquorice tablets. Methods:The analysis was performed by HPLC-ESI-MSMS. The acquisition was MRM ( multi-reaction monitor) , the column wasAgilentZorbaxEclipseSBC18(2.1mm×100mm,3.5 μm),themobilephasewasacetonitrileand15mmol·L-1ammoniumac-etate with gradient elution. Results:The precursor (m/z) of morphine and codeine was 286. 0 and 300. 0, respectively, and the quan-titative ion was 165. 0 and 165. 0, respectively. The linearity of morphine was excellent between 25 and 500ng·ml-1 , and the average recovery was 103. 1%. The linearity of codeine was good between 0. 75 ng and 150 ng·ml-1 , and the average recovery was 101. 5%with RSD of 1. 7(n=6). Conclusion:The method is simple and accurate, which can be used for the quality control of compound ligu-orice tablets.
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ABSTRACT BACKGROUND AND OBJECTIVES: Nonsteroidal anti-inflammatory drugs (NSAIDs) are frequently used to control arthroscopic pain. Addition of oral effective opioid "codeine" to NSAIDs may be more effective and decrease parenteral opioid consumption in the postoperative period. The aim of this study was to compare the efficacy and side effects of naproxen sodium and a new preparation naproxen sodium-codeine phosphate when administered preemptively for arthroscopic meniscectomy. METHODS: Sixty-one patients were randomized into two groups to receive either oral naproxen sodium (Group N) or naproxen sodium-codeine phosphate (Group NC) before surgery. The surgery was carried out under general anesthesia. Intravenous meperidine was initiated by patient-controlled analgesia (PCA) for all patients. The primary outcome measure was pain score at the first postoperative hour assessed by the Visual Analogue Scale (VAS). Sedation assessed by Ramsey Sedation Scale, first demand time of PCA, postoperative meperidine consumption, side effects and hemodynamic data were also recorded. RESULTS: The groups were demographically comparable. Median VAS scores both at rest and on movement were significantly lower in Group NC compared with Group N, except 18th hour on movement (p < 0.05). The median time to the first demand of PCA was shorter in Group N compared with Group NC (p < 0.001). Meperidine consumption was higher in Group N compared with Group NC (p < 0.001). There was no difference between groups with respect to side effects (p > 0.05). CONCLUSIONS: The combination of naproxen sodium-codeine phosphate provided more effective analgesia than naproxen sodium and did not increase side effects.
RESUMO JUSTIFICATIVA E OBJETIVOS: Os anti-inflamatórios não esteroides (AINEs) são frequentemente usados para controlar a dor após artroscopia. A adição de um opiáceo oral eficaz (codeína) aos AINEs pode ser mais efetiva e diminuir o consumo de opiáceo parenteral no pós-operatório. O objetivo deste estudo foi comparar a eficácia e os efeitos colaterais de naproxeno sódico e uma nova preparação, naproxeno sódico-fosfato de codeína, quando administrados preventivamente para meniscectomia artroscópica. MÉTODOS: Foram randomicamente divididos em dois grupos 61 pacientes para receber naproxeno sódico por via oral (Grupo N) ou naproxeno sódico-fosfato de codeína (Grupo NC) antes da cirurgia. A cirurgia foi feita sob anestesia geral. Meperidina intravenosa foi iniciada por meio de analgesia controlada pelo paciente (ACP) para todos os pacientes. O desfecho primário foi o escore de dor na primeira hora de pós-operatório, avaliada com a escala visual snalógica (EVA). A sedação foi avaliada com a escala de sedação de Ramsey. A primeira demanda de ACP, o consumo de meperidina no pós-operatório, os efeitos colaterais e os dados hemodinâmicos também foram registrados. RESULTADOS: Os grupos foram demograficamente comparáveis. As medianas dos escores EVA tanto em repouso quanto em movimento foram significativamente menores no Grupo NC comparado com o Grupo N; exceto para movimento na avaliação de 18 horas (p < 0,05). A mediana do tempo até a primeira demanda de ACP foi menor no Grupo N em comparação com o Grupo NC (p < 0,001). O consumo de meperidina foi maior no Grupo N em comparação com o Grupo NC (p < 0,001). Não houve diferença entre os grupos em relação aos efeitos colaterais (p > 0,05). CONCLUSÕES: A combinação de naproxeno sódico-fosfato de codeína forneceu analgesia mais efetiva que naproxeno sódico, sem aumentar os efeitos colaterais.
Subject(s)
Humans , Male , Female , Adult , Arthroscopy/methods , Naproxen/administration & dosage , Codeine/administration & dosage , Meniscus/surgery , Pain, Postoperative/drug therapy , Pain Measurement , Anti-Inflammatory Agents, Non-Steroidal/administration & dosage , Anti-Inflammatory Agents, Non-Steroidal/adverse effects , Naproxen/adverse effects , Double-Blind Method , Prospective Studies , Follow-Up Studies , Analgesia, Patient-Controlled/methods , Codeine/adverse effects , Drug Combinations , Analgesics, Opioid/administration & dosage , Meperidine/administration & dosage , Middle AgedABSTRACT
To establish a method for the simultaneous determination of the active ingredients ( codeine phosphate, brompheniramine maleate, chlorpheniramine maleate, ephedrine hydrochloride and guaifenesin) in compound codeine phosphate oral preparations by capillary electrophoresis ( CE) . Methods:The method employed an uncoated capillary column ( eCAPTM ) from Beck-mann company (50 cm × 75 μm);the electrophoresis voltage was at 10 kV;20 mmol·L-1 phosphate buffer solution (pH 7. 5) was used;the UV measurement was at the wavelength of 214 nm. Results: The studied components had good linear ranges (r≥0. 995) within the range of the investigated concentrations. The recovery was no less than 96%. Conclusion:The presented method can be ap-plied in the content determination of active ingredients in compound codeine phosphate oral preparations from different enterprises. It is simple, efficient and universal, which facilitates the market supervision in a fast and valid manner.
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Objective To investigate the effect and safety of Compound codeine phosphate syrup with Ambroxol treatment in the stable phase of chronic obstructive pulmonary disease. Methods 100 patients with stable COPD were divided into Compound codeine phosphate syrup with Ambroxolt treatment group (Group A) 50 cases and Compound codeine phosphate syrup treatment group( Group B) 50 cases,drug were given for 3 ～ 7d. The symptom score and efficacy of two groups before treatment and after treatment were compared. Results The symptom score of cough,sputum volume,sputum viscosity ,wheeze,sleep after treatment 8th day were improved significantly ( χ2 = 3. 891 ,χ2 =3. 992, χ2 = 4. 198, χ2 = 3.981, χ2 = 3. 879, allP < 0. 05; Total effective rate of cough, sputum volume, sputum viscosity,wheeze in group A(92. 0% ,94. 0% ,90. 0% ,90. 0% ) higher than that in group B(80.0% ,86.0% ,80. 0%,78.0% ) ( χ2 = 3.991, χ2 = 4. 012, χ2 = 3. 998, χ2 = 3.971, allP < 0. 05); The adverse reactions of A、 B group were 12.0% and 14.0%(χ2 =1.971,P>0.05). Conclusion Compound codeine phosphate syrup with Ambroxol is an effective and safe antitussive in the stable phase of chronic obstructive pulmonary disease.
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Objective To establish a novel method for simultaneous determination of three ingredients (codeine phosphate, brompheniramine maleate and ephedrine hydrochloride) in compound codeine phosphate solution by using capillary electrophoresis (CE) coupled with electrochemiluminescence (ECL). Methods Based on enhanced ECL intensity of tris (2,2′-bypyridine) ruthenium (Ⅱ) with codeine phosphate, brompheniramine maleate and ephedrine hydrochloride, as well as the linear correlation between enhanced sensitivity intensity and drug concentration, Parameters affecting separation and detection were optimized. Results Under the optimized conditions, we determined the linear range, regression equation and detection limit for the three ingredients. The relative standard deviation of ECL intensity for twelve consecutive injections of 1.0×10~(-5)kg/L standard sample of three kinds of drug was 2.89% for codeine phosphate, 3.76% for brompheniramine maleate and 3.32% for ephedrine hydrochloride, respectively. Satisfactory results were obtained without interference from sample matrixes. Conclusion The method was successfully applied to the determination of three ingredients in oral solution of compound codeine phosphate, with the recovery rate of 100.4% for codeine phosphate, 101.9% for brompheniramine maleate and 99.8% for ephedrine hydrochloride.
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OBJECTIVE:To evaluate the clinical efficacy and safety of guaifenesin,pseudoephedrine hydrochloride- codeine phosphate oral solution in relieving cough,eliminating phlegm,relieving nasal stuffiness and other cold symptoms. METHODS:A total of 240 patients with cold symptoms(120 cases in trial group and another 120 cases in control group) were enrolled in our multicenter,randomized,double-blinded and parallel controlled study and treated with guaifenesin-pseudoephedrine hydrochloride-codeine phosphate oral solutionI or compound codeine phosphate liquor 10mL tid for(5?2)d.RESULTS:227(112 in trial group and 115 in control group) were the valid cases with completed trial.Compared with pre-treatment,both of the 2 groups had a significant improvement in symptoms including cough,expectoration and nasal stuffiness after treatment(P