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OBJECTIVE：To es tablish a method for the content determination of heavy metals [lead （Pb），cadmium（Cd）， copper （Cu）， mercury （Hg）] and harmful elements [arsenic （As）] in Pediatric paracetamol artificial cow-bezoar and chlorphenamine maleate granules. METHODS ：The samples were conducted pretreatment by microwave digestion instrument and determined by inductively coupled plasma mass spectrometry （ICP-MS）using elements germanium ，indium，bismuth as internal standard. RESULTS ：The linear ranges of Pb ，As，Cu，Cd and Hg were 1-20，0.5-10，5-100，0.5-10 and 0.2-4 ng/mL， respectively （all r＞0.997）. The limits of detection （LODs） were 0.041 1，0.013 2，0.057 3，0.009 0，0.005 4 ng/mL， respectively. The limits of quantification （LOQs）were 0.137 0，0.044 0，0.191 0，0.030 0，0.018 0 ng/mL，respectively. RSDs of precision and repeatability tests were all less than 6％. RSDs of stability tests （28 h）of Pb ，As，Cu and Cd were all less than 5％， and that of stability test （28 h）of Hg was less than 7％. The average recoveries were 89.44％（RSD＝5.87％，n＝9），99.56％ （RSD＝5.46％ ，n＝9），96.12％（RSD＝4.62％ ，n＝9），105.82％（RSD＝2.80％ ，n＝9）and 90.23％（RSD＝3.59％ ，n＝9）， respectively. Five elements were all detected in 63 batches of samples ，and the contents of them were 0.191 0-1.527 6，0.002 5- 0.047 4，0.034 1-1.549 0，0.001 5-0.078 8 and 0.001 9-0.005 4 mg/kg，respectively. CONCLUSIONS ：The method is simple ， sensitive and accurate. It is suitable for simultaneous determination of 5 elements in Pediatric paracetamol artificial cow-bezoar and chlorphenamine maleate granules.
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OBJECTIVE:To establish the method for simultaneous contents determination of 5 kinds of acid and alkaline componentsin anti-cold compound preparation. METHODS:HPLC method was adopted. The workstation was Auto·Blend Plus software of ACQUITY Arc system. The determination was performed on Discovery?HS F5-5 column with mobile phase consisted of acid mixture-base mixture-methanol-0.3% triethylamine (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelengths were set at 270 nm (acetaminophen,salicylamide,chlorphenamine maleate,triprolidine hydrochloride) and 299 nm (aspirin). The column temperature was 35 ℃,the sample size was 20 μ L. RESULTS:The linear ranges of acetaminophen, salicylamide,acetylsalicylic acid,chlorphenamine maleate,triprolidine hydrochloride were 26-411 μ g/mL(r＝0.999 6),16-254 μg/mL(r＝0.999 8),16-748 μg/mL(r＝0.998 1),35-565 μg/mL(r＝0.999 8)and 25-404 μg/mL(r＝0.999 7),respectively. LOQ were 3.6,3.1,4.0,9.6,6.3 μ g/mL;LOD were 1.9,1.3,1.4,2.9,2.3 μ g/mL,respectively. RSDs of intermediate precision, stability and reproducibility tests were all lower than 2%. Average recoveries were 100.0%-102.0%(RSD＝0.59%,n＝9), 95.2%-101.0%(RSD＝1.55%,n＝9),96.2%-99.9%(RSD＝1.24%,n＝9),96.2%-101.5%(RSD＝1.57%,n＝9),96.3%-98.9%(RSD＝0.83%,n＝9),respectively. RSDs of durability tests were lower than 3%. CONCLUSIONS:The method is simple, accurate,precise,stable,reproducible and durable,and can be used for simultaneous contents determination of 5 kinds of acid and alkaline components in anti-cold compound preparation.
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OBJECTIVE:To establish a method for the simultaneous determination of paracetamol,amantadine hydrochloride, caffeine,chlorphenamine maleate in Compound paracetamol and amantadine hydrochloride tablet. METHODS:GC was performed on the column of HP-5 sillica capillary,temperature programmed,detector was FID detector,with the temperature of 300 ℃,car-rier gas was nitrogen gas,the flow rate is 1.5 mL/min,the split ratio was 20:1 and injection volume was 1μL. RESULTS:The lin-ear range was 156.0-4990.4 μg/mL for paracetamol,125.7-4023.2 μg/mL for amantadine hydrochloride,19.14-612.4 μg/mL for caffeine and 2.515-80.48 μg/mL for chlorphenamine maleate(all r=0.9999);the limits of quantification were 1.4,0.5,1.1,0.9 ng,limits of detection were 0.4,0.2,0.3,0.3 ng;RSDs of precision,stability and reproducibility tests were lower than 2.0%;re-coveries were 99.59%-101.77%(RSD=0.8%,n=9),99.56%-101.80%(RSD=0.7%,n=9),98.44%-100.83%(RSD=0.7%,n=9) and 100.05%-101.91%(RSD=0.6%,n=9),respectively. CONCLUSIONS:This method is simple,rapid,accurate and reli-able,and suitable for the simultaneous determination of paracetamol,amantadine hydrochloride,caffeine,chlorphenamine maleate in Compound paracetamol and amantadine hydrochloride tablet.
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Objective: Combining with national drug sampling program,to evaluate the current quality situation and problems of compound Yinqiao and paracetamol and chlorphenamine maleate capsules by testing and analyzing 78 batches of samples collected from the realm of drug production and circulation all over the country in 2015.Methods: As the current standard could not control the product quality, and combined the prescribed examination with exploratory research, the method of HPLC was used to determine the contents.GC and TLC was respectively used to identify peppermint oil and study on forsythin.Near infrared spectrum database was established by near-infrared spectroscopy (NIRS), which provided the basis for rapid testing.The results of the prescribed examination and exploratory research were statistically analyzed.Results: There were significant differences in the results of the prescribed examination and exploratory research.Conclusion: The results of exploratory research show that there are many defects in the statutory standards.The product quality of different manufactures was divers, and it is necessary to guide them to improve the preparation process and the quality.More exclusive, accurate and sensitive methods should be used to comprehensively control the quality.
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Objective:To compare the dissolution of compound fructus forsythiae, paracetamol and chlorphenamine maleate cap-sules from different manufacturers.Methods: The dissolution test was carried out by a basket method in 900 ml dissolution medium with the rotating speed at 100 r·min-1. The dissolution profiles of compound fructus forsythiae,paracetamol and chlorphenamine mal-eate capsules from different manufacturers in four dissolution media including hydrochloric acid solution, pH 4.5 acetate buffer solu-tion,water and pH 6.8 phosphate buffer solution were determined,and the dissolution curves were compared by a similar factor meth-od. Results:The cumulative dissolution of compound fructus forsythiae,paracetamol and chlorphenamine maleate capsules from seven manufacturers was all over 70% in 30 min in hydrochloric acid solution,while failed to dissolve well in pH 4.5 acetate buffer solution, water and pH 6.8 phosphate buffer solution. All the dissolution curves in the 4 dissolution media were different among the batches. Conclusion:The quality of compound fructus forsythiae,paracetamol and chlorphenamine maleate capsules from various manufacturers is much different. Promising dissolution should be guaranteed,at the same time,the stability needs to be improved.
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OBJECTIVE:To investigate the application of fuzzy comprehensive evaluation in formulation screening. METH-ODS:Taking Compound paracetamol and chlorphenamine maleate granules as model drug,based on single factor experiment,L9(34) orthogonal test was used to screen the formulation with the amount of aspartame,hawthorn powder essence,milk powder essence and saccharose as factors,using dissolution rate of caffeine as index. The granules prepared by 9 kinds of formulation in orthogonal test were evaluated with fuzzy comprehensive evaluation in terms of taste,aroma,color and dissolubility. The optimized formula-tion was validated and compared with original formulation. RESULTS:The formulation 5 was the optimal choice in both orthogo-nal test and fuzzy comprehensive evaluation,and obtained same results. Compared with sensory comprehensive score (63.12) and dissolution rate of caffeine (91.3%) in original formulation,two indicators of optimized formulation in 3 tests were 84.00 and 99.07% in average (RSD<2.0%,n=3). CONCLUSIONS:Fuzzy comprehensive evaluation can be used for the formulation screening of sensory evaluation index. It is scientific and accurate.
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Objective:To establish a method for the simultaneous determination of chlorphenamine maleate and ephedrine hydro-chloride in chlorphenamine maleate and ephedrine nasal drops by HPLC. Methods:An HPLC method was performed on a column of Purospher STAR RP18(150 mm × 4. 6 mm,5 μm)with the mobile phase of acetonitrile -potassium dihydrogen phosphate buffer(pH 3. 0 ± 0. 1)(18:82 v/v)at the detection wavelength of 210 nm(adjusting the flow rate and column temperature to 1. 0 ml·min-1 and 35℃,respectively). The injection volume was 20 μl. Results:A good linear relationship was established between the peak response and the concentration of ephedrine hydrochloride and chlorphenamine maleate over the range of 19. 81-118. 85μg·ml-1(r=0. 999 6) and 6. 21-37. 25 μg·ml-1(r=0. 999 8),respectively. The mean recovery of ephedrine hydrochloride and chlorphenamine maleate was 100. 39%(RSD=0. 69%,n=9)and 100. 11%(RSD=0. 60%,n=9),respectively. Conclusion:The proposed method shows high repeatability,good durability and promising accuracy. It can be employed for the determination of two components in chlorphena-mine maleate and ephedrine nasal drops.
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Objective:To unify the content determination method for chlorphenamine maleate tablets and injections. Methods:An Inertsil C8(150 mm × 4. 6 mm,5 μm)column was used,the mobile phase was phosphate buffer( ammonium phosphate monobasic 11. 5g was dissolved in water,1 ml phosphoric acid was added and diluted to 1 000 ml by water)-acetonitrile(70:30),the flow rate was 1. 0 ml·min-1 ,the column temperature was room temperature,the sample volume was 10 μl and the detection wavelength was 262 nm. Results:The linear range of chlorpheniramine was 0. 017 8-0. 445 0 mg·ml-1(r=0. 999 9);the average recovery of the tablets and injections was 100. 2%(RSD=0. 4%,n=9)and 100. 3%(RSD=0. 9%,n=9),respectively. Conclusion:The method is simple,reproducible and accurate,and can provide reliable basis for the standards of chlorpheniramine maleate tablets,injections and dropping pills.
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Objective:To establish an HPLC method for the determination of p-aminophenol in pediatric paracetamol artificial cow-bezoar and chlorphenamine maleate granules. Methods: A CAPCELL PAK MGⅡC18 (150 mm × 4. 6 mm,5 μm) chromatographic column was used with 0. 05% ammonium acetate solution-methyl (85∶ 15) as the mobile phase at the flow rate of 1 ml·min-1 , the detection wavelength was 232nm,the injection volume was 10μl,and the column temperature was 30℃. Results:The linear range of p-aminophenol was 9. 878 4-197. 568 0 ng(r = 0. 999 1), the average recovery was 99. 8%(RSD = 0. 9%,n= 9), and detection limit was 2ng. Conclusion:The method is simple, specific and accurate, which can be used to determine the contents related substances in of pediatric paracetamol artificial cow-bezoar and chlorphenamine maleate granules.
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OBJECTIVE:To establish a method for the bacterial endotoxin test of chlorphenamine maleate injection. METHODS: The interference test and bacterial endotoxin test of 28 batches of chlorphenamine maleate injections from 14 manufacturers were carried out in accordance with the bacterial endotoxin test approved by Chinese Pharmacopeia (2005 edition). RESULTS: Diluted to a concentration of below 0.025 mg?mL-1,the samples showed no interference action on bacterial endotoxin test. The limit value of the bacterial endotoxin was 5 EU?mg-1. The results of the bacterial endotoxin test of the 28 batches of samples were all accorded with the standard of the established quality control. CONCLUSION: The established TAL method is applicable for bacterial endotoxin test of chlorphenamine maleate injection.
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OBJECTIVE:To compare the in vitro dissolubility of four kinds of commercial chlorphenamine maleate tablets. METHODS: To determine the dissolubility of four kinds of domestic commercial chlorphenamine meleate tablets by paddle method and to analyse the dissolution parameters, T50, Td, m, by variance analysis method. RESULTS: The dissolution parame- ters of the different tablets were T50(30. 3 197, 17. 3 695, 20. 1038, l4. 3 651), Td(34. 6 088, 26. 7 162, 28. 0 514, 22. 1 593)and m (2. 7 676, 0. 8 505, 1. 0 992, 0. 8 448). CONCLUSION: The statistical results indicated that there were significant differences between them(P
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Objective: To establish a method for the determination of metamizole sodium and chlorphenamine malete in zhongganling Tablets. Methods: The sample was determined by ion pair HPLC after it was purified on Sep Pak C 18 microcolumn. The chromatographic conditions included: Hypersil DBS C 18 chromatographic column (250mm?4.6mm, i.d.5?m) as an anlaytical column, methanol mixed solution of sodium heptanesulfonate and glacial acetic acid (600∶400) as a mobile phase, the detection wavelength at 264nm and 1.0mL?min -1 of flow rate. Results: The average recoveries of metamizole sodium and chlorphenamine maleate were 99.6% (RSD was 2.1% and n was 6) and 98.0% (RSD was 1.5% and n was 6), respectively. Conclusion: Metamizole sodium and chlorphenamine maleate can be determined respectively by HPLC with the same mobile phase when Sep Pak C 18 microcolumn solid phase extraction method is used to substitute for the traditional sample pretreatment methods refluxing, extracting and concentrating, and sodium heptanesulfonate ion pair reagent in acid condition is selected.
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AIM:To establish a method of determining the content of chlorogenic acid,paracetmol,vitamin C and chlorphenamine maleate in Vitamin C Yinqiao Tablets. METHODS: The separation was performed in the C_(18) colunm with the mobile phase of methanol-acetonitril-0.02% phosphate acid(5∶10∶85).The flow rate was(1.0 mL/min) with the wavelength at 219 nm and 310 nm,the temperature of column was 35 ℃. RESULTS: The calibration curves were linear in the ranges of 0.03-0.13 ?g for chlorogenic acid,0.94-4.68 ?g for paracetmol,0.49-2.44 ?g for Vitamin C,0.01-0.05 ?g for chlorphenamine maleate,the average recoveries were not less than 98%,respectively. CONCLUSION: The method is simple,rapid and with satisfactory results.It is suitable for quality control of Vitamin C Yinqiao Tablets.
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Objective: To establish the quality standard for Ganmaoling Tablets (Radix Ilex asprella, Flos Chrysanthem Indici, Ramulus et Radix Evodia leptae, acetaminophe, etc.). Methods:The acetaminophen, chlorphenamini maleas, caffeine, Radix Ilex asprella, Flos Chrysanthem Indici, Ramulus et Radix Evodia leptae were identified by TLC. The acetaminophen and chlorogenic acid were determined by HPLC. Results:The average recovery of acetaminophe was 101.36%, and RSD was 0.93%, respectively. The average recovery of chlorogenic acid was 100.8%, and RSD was 0.9%, respectively. Conclusion:The method developed is accurate and the reproducibility is good. The method can be used for quality control of the Ganmaoling Tablets.