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Objective:To establish a headspace GC method for the determination of residual formaldehyde in EDTA-2Na. Meth-ods:A headspace GC was used to separate the residual solvents on an Agilent DB-WAX (30 m×0.32 mm,0.5 μm) capillary col-umn with an FID detector. The carrier gas was nitrogen at the flow rate of 1.0 ml·min-1. The temperature of the injector was 230 ℃and that of the FID was 260 ℃. The programmed column temperature was set as follows: maintained at 40 ℃ for 6 min, and then raised to 230 ℃ at the rate of 40 ℃·min-1and maintained for 10 min. The injection volume was 1μl with the split ratio of 2:1. The reference solvent and sample were filled into the containers of headspace injector and the containers were in equilibrium at 95℃ for 25 min. The amount of residual formaldehyde was calculated by an external standard method.Results:There was a good linear relationship of formaldehyde reference solvent within the concentration range of 5.10-102.00 μg·ml-1(r=0.999 7). The average recovery was 84.60%(RSD=3.82%,n=9). Conclusion: The method is simple,rapid and accurate for the determination of residual formalde-hyde in EDTA-2Na.
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Objective:To determine the phase-transition temperature of white vaseline produced by different processes by differen-tial scanning calorimetry ( DSC) in order to analyze the relevance between the melting point and the phase-transition temperature and the relevance between different production processes and the phase-transition temperature. Methods: Hermertic aluminum pans were used to encapsulate the samples, and the testing conditions were optimized. The sample weight was about 10 mg, and the range of measuring temperature was -20-100℃. The heating rate was 5℃·min-1 and the flow rate of nitrogen was 30 ml·min-1 . Results:The phase-transition temperature and the melting point were significantly different. The phase-transition temperature of white vaseline samples produced by different processes was quite different. Conclusion:Melting point determination in the current standard method of white vaseline exists defects, and the composition of white vaseline produced by various processes is quite different.
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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 analyze the compatibility rationality between the raw material and auxiliary material sodium bisulfite in Zhengqin Fengtongning injection.Methods: HPLC was applied to detect the contents of the impurity and the main component in Zhengqing Fengtongning injection, and ion chromatography was applied to determine the content of sodium bisulfite in Zhengqing Fengtongning injection.The changes of impurity, main component and sodium bisulfite among the samples were compared before and after the stress testing (high temperature at 40℃, 60℃ and illumination at 4 500 lx).LC-MS-MS was used to identify the structures of the impurities.Results: The impurity in Zhengqing Fengtongning injection was the combination of the raw material and sodium bisulfite.Conclusion: It is irrational for Zhengqing Fengtongning injection to use sodium bisulfite as the antioxidant.
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Objective: To improve the quality standard for Zengguang tablets.Methods: Instead of the microscopic identification, Acorus tatarinowii rhizoma,Lycii Fructus and Polygalae radix were indentified by TLC.The content of schisandrin in Schisandrae Chinensis Fructus was determined by HPLC.The HPLC system consisted of a Hypersil BDS C18(250 mm×4.6 mm,5 μm)column, methanol-water (1∶1) was used as the mobile phase at a flow rate of 1.0 ml·min-1, and the detection wavelength was at 250 nm.The column temperature was 35℃ and the sample size was 10 μl.Results: The microscopic images were with strong specificity.The developed TLC spots were quite clear, and the method of TLC was simple with strong specificity and good reproducibility.The linear range of schisandrin was 21.17-423.40 ng(r=0.999 9).The average recovery was 99.7% and the RSD was 1.4%(n=6).Conclusion: The method for the quality control of Zengguang tablets is comprehensive and perfect.
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Objective:To compare the quality differences in benzalkonium chloride samples from domestic and abroad to provide references for the quality standard revision for benzalkonium chloride in Chinese pharmacopoeia. Methods: The ratio of alkyl compo-nents was determined according to the method described in USP 38, and the total content of benzalkonium chloride was determined ac-cording to the method recorded in Chinese Pharmacopoeia (2015 edition) and USP 38, respectively. Results:According to the results of composition ratio of alkyl, the fraction defective of domestic samples and imported samples was 100% and 50%, respectively. The content difference between the values calculated by the methods in the two pharmacopoeias showed that the total content of domestic samples changed from 3. 86% to 4. 15%, and that of imported samples changed from 1. 15% to 3. 90%. Conclusion:There are sig-nificant differences in the quality of benzalkonium chloride between domestic samples and imported samples. It is recommended that the ratio of alkyl components should be supplemented in our pharmacopoeia referring to the method in USP 38 and the total content calcula-tion formula for benzalkonium chloride should be revised to improve the quality standard for benzalkonium chloride.
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OBJECTIVE:To establish a method to determine and compare the contents of sodium benzoate in medicinal(phar-maceutical excipients and active pharmaceutical ingredients) and non-medicinal (chemical reagents and food additives) grade. METHODS:HPLC was conducted for content determination,SPSS 18.0 software was adopted to compare the results. The column was Purospher STAR LP RP-18 endcapped with mobile phase of acetotrile-0.02% formic acid(adjusted pH to 4.0 with aqua ammo-nia)(30∶70,V/V)at a flow rate was 1.0 ml/min,the detection wavelength was 230 nm,column temperature was 35 ℃,and vol-ume injection was 20 μl. RESULTS:The linear range of sodium benzoate was 10.5-525.3 μg/ml(r=0.999 9);RSDs of precision, stability,reproducibility and durability tests were lower than 0.5%;recovery was 99.38%-101.26%(RSD=0.56%,n=9). The av-erage contents of sodium benzoate in medicinal and non-medicinal grade were between 99.400%-99.875%,but the average content of non-medicinal grade is lower than the medical grade. CONCLUSIONS:The method is accurate and simple with high specificity and good reproducibility,and can be used to determine and compare the content of sodium benzoate in medicinal and non-medici-nal grade.
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Objective:To determine the related substances in benzalkonium chloride used as a pharmaceutical adjuvant, and com-pare the quality at home and abroad. Methods:An HPLC method was used with an ODS-HYPERSIL C18 column(250 mm × 4. 6 mm, 5 μm). The detection wavelength was 210 nm and 257 nm. The flow rate was 1. 0 ml· min-1 and the column temperature was 30℃. The injection volume was 20 ml. The mobile phase was A ( dissolving 1. 09 g sodium1-hexanesulfonate and 6. 9 g sodium dihydrogen phosphate in water, adjusting pH to 3. 5 with phosphoric acid and diluting to 1 000. 0 ml) and B ( methanol) with gradient elution. Results:The content of benzaldehyde in the samples at home and abroad was low. The content of benzyl alcohol in the samples from a-broad was qualified, which was significantly higher than that in the domestic samples. The content of benzyl chloride in the domestic samples was higher than that in the samples from abroad. Conclusion:The method is simple and fast, which is suitable for comparing the related substances of domastic and imported samples. At the same time, the study provides basis for enterprises to choose benzalko-nium chloride rationally.
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Objective:To establish the method for determining the related substances in lansoprazole for injection and qualitatively study the impurities. Methods:An HPLC method and an HPLC-MS method were used with isocratic elution and DAD as the detector. Results:The priciple impurity in all samples was impurity B. Conclusion:The method is fast, simple and sensitive, and suitable for the determination of the related substances in lansoprazole for injection.
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Objective: To determine the impurities in pharmaceutical adjuvant sodium bisulfite. Methods: An IC method was used with a Dionex IonPac AS17-C RFIC analytical column. ECD was used as the detector by gradient elution and the temperature of column was 30℃. Results:Sulfate radical was detected out in all samples. Conclusion:The method is simple and fast with high sensi-tivity, which is suitable for the determination of related substances in sodium bisulfite.
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OBJECTIVE@#To determine the correlation among the levels of C-reactive protein (CRP) and interleukin-18 (IL-18), quality of life, and pulmonary function in patients with chronic obstructive pulmonary disease (COPD),and to evaluate George's respiratory questionnaire (SGRQ).@*METHODS@#From October 2008 to March 2009, 39 patients with an acute exacerbation COPD (the AECOPD group), 21 patients with stable COPD (the COPD group), and 22 normal people (the control group) were enrolled in our study. The serum CRP level was measured with Beckman Coulter Immage and the IL-18 level was measured by ELISA. All subjects completed the SGRQ assessment and all patients with COPD accepted pulmonary function test.@*RESULTS@#The serum levels of CRP and IL-18, and SGRQ scores in the AECOPD group were significant1y higher than those in the COPD group and the control group (P<0.01). The serum levels of CRP and IL-18 and SGRQ scores in the COPD group were significant1y higher than those in the control group (P<0.01). The serum levels of CRP and IL-18 in the AECOPD group and the COPD group were negatively correlated with FEV1% and forced expiratory volume in one second (FEV1)/forced vital capacity (FVC). SGRQ scores in the AECOPD group and the COPD group were negatively correlated with FEV1% and FEV1/FVC. The serum levels of CRP, IL-18 in the AECOPD group and the COPD group were positively correlated with SGRQ scores.@*CONCLUSION@#CRP and IL-18 are involved in the process of inflammatory reaction of COPD, which could be markers of the acute exacerbation period of COPD. The serum levels of CRP and IL-18 might be related to the lung dysfunction and the lower quality of life in the patients with COPD. SGRQ is an effective, susceptible, and feasible method to evaluate the quality of life in patients with COPD.
Subject(s)
Aged , Female , Humans , Male , Middle Aged , C-Reactive Protein , Metabolism , Case-Control Studies , Forced Expiratory Volume , Interleukin-18 , Blood , Lung , Pulmonary Disease, Chronic Obstructive , Blood , Quality of Life , Respiratory Function Tests , Surveys and Questionnaires , Vital CapacityABSTRACT
Objective To develop the method for determining the content of Schisandrin by HPLC. Method The Schisandrin in Hugan Pill was determinined by HPLC. The analytical column was Hanbon Lichrospher (250 mm?4.6 mm, 5 ?m) and mobile phase was methanol-water (67∶33), with wavelength was set at 251 nm. Result Schisandrin had good linear relationship with their peak area in the range of 0.105 1～2.102 ?g (r=0.999 9, n =7). The average recovery rate was 97.03%, RSD was 1.02% (n =5). Conclusion The method was rapid, simple and precise.