HPLC法测定复方苯甲酸软膏中苯甲酸和水杨酸的含量
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摘要
目的建立梯度洗脱的高效液相色谱法(HPLC)法,测定复方苯甲酸软膏中苯甲酸、水杨酸的含量。方法采用HPLC,色谱柱为Diamonsil C18,以甲醇-0.1%磷酸溶液(45:55)为流动相,波长230nm,流速1.0ml/min,柱温40℃,进行试验。结果苯甲酸、水杨酸分别在2.11～37.98μg/ml和1.99～35.84μg/ml范围内,其与峰面积线性关系较好;精密度、稳定性和重复性实验的相对标准偏差(RSD)均<0.30%;苯甲酸和水杨酸平均加样回收率分别为100.07%和100.01%,RSD分别为0.55%和0.51%。结论 HPLC法测定复方苯甲酸软膏中苯甲酸、水杨酸含量,具有准确、快速、重复性好等优点。
Objective The contents of benzoic acid and salicylic acid in compound benzoic acid ointment were determined by high performance liquid chromatograph(HPLC) method with gradient elution. Methods HPLC were used,the chromatographic column was Diamonsil C18,the mobile phase was methanol-0.1% phosphoric acid solution(45:55),the detection wavelength was230 nm,the velocity was 1.0ml/min,and the column temperature was 40℃. Results Benzoic acid in 2.11～37.98μg/ml and salicylic acid in 1.99～35.84μg/ml range had good linear relationship with peak area;All the relative standard deviation(RSD),stability and repeatability of the experiment were less than 0.30%;The average recovery rates of benzoic acid and salicylic acid were 100.07%and 100.01%,respectively,and RSD were 0.55% and 0.51%,respectively. Conclusion The HPLC method is used to determine the content of benzoic acid and salicylic acid in compound benzoic acid ointment,and this method has the advantages of accurate,rapid,reproducible.
Objective The contents of benzoic acid and salicylic acid in compound benzoic acid ointment were determined by high performance liquid chromatograph(HPLC) method with gradient elution. Methods HPLC were used,the chromatographic column was Diamonsil C18,the mobile phase was methanol-0.1% phosphoric acid solution(45:55),the detection wavelength was230 nm,the velocity was 1.0ml/min,and the column temperature was 40℃. Results Benzoic acid in 2.11～37.98μg/ml and salicylic acid in 1.99～35.84μg/ml range had good linear relationship with peak area;All the relative standard deviation(RSD),stability and repeatability of the experiment were less than 0.30%;The average recovery rates of benzoic acid and salicylic acid were 100.07%and 100.01%,respectively,and RSD were 0.55% and 0.51%,respectively. Conclusion The HPLC method is used to determine the content of benzoic acid and salicylic acid in compound benzoic acid ointment,and this method has the advantages of accurate,rapid,reproducible.
引文
[1]李秀敏,赵颖,杨宁,等.海勒氏液中苯甲酸、水杨酸的含量测定[J].药物分析杂志,2015,13(11):2032-2035.
[2]张媛媛,郝光涛,董瑞华,等.HPLC-MS/MS法同时测定人血浆中舒尼替尼及其活性代谢产物SU12662的浓度[J].中国临床药理学杂志,2015,19(23):2348-2351.
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[4]时正媛,曾蔚欣,杨丽,等.双波长HPLC法同时测定复方水杨酸甲酯软膏中盐酸麻黄碱和水杨酸甲酯的含量[J].中国药房,2015,24(3):369-371.
[5]田莉,张仁正,李静峰,等.HPLC法测定熟肉制品中苯甲酸、山梨酸和脱氢乙酸的含量[J].中国食品添加剂,2016,22(10):172-175.
[6]孟素蕊,焦建杰,高洋,等.HPLC法测定小鼠血清中的4-甲基-3-硝基苯甲酸及药动学研究[J].药物分析杂志,2015,11(2):273-277.
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[8]刘彦,倪美萍,刘睿思,等.中药口服液中苯甲酸、山梨酸和糖精钠的中空纤维离心超滤-HPLC法测定[J].中国医药工业杂志,2017,31(5):726-729.
[9]Chung IM,Lim JJ,Ahn MS,et al.Comparative phenolic compound profiles and antioxidative activity of the fruit,leaves,and roots of Korean ginseng(Panax ginseng,Meyer)according to cultivation years[J].J Ginseng Res,2016,40(1):68-75.
[10]胡军红,谢建红,邓灼斌,等.CLSI EP9-A3在两种不同方法测定糖化血红蛋白结果比对及偏倚评估中的应用[J].实验与检验医学,2018,36(2):188-190,192.
[11]Sisi Chen,Casey Burton,Anthony Kaczmarek,等.Simultaneous Determination of Urinary Quinolinate,Gentisate,4-Hydroxybenzoate,andα-Ketoglutarate by High-Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Anal Methodsuk,2015,7(16):6572-6578.
[12]孔燕凌.HPLC同时测定墨旱莲正丁醇有效部位含量分析[J].实验与检验医学,2017,35(4):475-478.
[13]Gliozzi G,Passeri S,Bortolani F,et al.Zeolite Catalysts for Phenol Benzoylation with Benzoic Acid:Exploring the Synthesis of Hydroxybenzophenones[J].Catalysts,2015,5(4):2223-2243.
[14]田莉,张炯怡,李静峰,等.HPLC法测定凉拌菜中苯甲酸、山梨酸和糖精钠的含量[J].中国调味品,2016,41(6):132-134.
[15]李向阳,高洁,屠万倩,等.RP-HPLC法测定逍遥丸(水丸)中芍药苷、苯甲酸和苯甲酰基总苷[J].中成药,2015,37(8):1722-1727.
[2]张媛媛,郝光涛,董瑞华,等.HPLC-MS/MS法同时测定人血浆中舒尼替尼及其活性代谢产物SU12662的浓度[J].中国临床药理学杂志,2015,19(23):2348-2351.
[3]姜爱霞,历娜.水杨酸苯酚贴膏中有关物质测定方法及应用[J].第三军医大学学报,2015,37(15):1599-1602.
[4]时正媛,曾蔚欣,杨丽,等.双波长HPLC法同时测定复方水杨酸甲酯软膏中盐酸麻黄碱和水杨酸甲酯的含量[J].中国药房,2015,24(3):369-371.
[5]田莉,张仁正,李静峰,等.HPLC法测定熟肉制品中苯甲酸、山梨酸和脱氢乙酸的含量[J].中国食品添加剂,2016,22(10):172-175.
[6]孟素蕊,焦建杰,高洋,等.HPLC法测定小鼠血清中的4-甲基-3-硝基苯甲酸及药动学研究[J].药物分析杂志,2015,11(2):273-277.
[7]Heydari R,Mousavi M.Simultaneous determination of saccharine,caffeine,salicylic acid and benzoic acid in different matrixes bysalt and air-assisted homogeneous liquid-liquid extraction and highperformance liquid chromatography[J].J Chil Chem Soc,2016,61(3):3090-3094.
[8]刘彦,倪美萍,刘睿思,等.中药口服液中苯甲酸、山梨酸和糖精钠的中空纤维离心超滤-HPLC法测定[J].中国医药工业杂志,2017,31(5):726-729.
[9]Chung IM,Lim JJ,Ahn MS,et al.Comparative phenolic compound profiles and antioxidative activity of the fruit,leaves,and roots of Korean ginseng(Panax ginseng,Meyer)according to cultivation years[J].J Ginseng Res,2016,40(1):68-75.
[10]胡军红,谢建红,邓灼斌,等.CLSI EP9-A3在两种不同方法测定糖化血红蛋白结果比对及偏倚评估中的应用[J].实验与检验医学,2018,36(2):188-190,192.
[11]Sisi Chen,Casey Burton,Anthony Kaczmarek,等.Simultaneous Determination of Urinary Quinolinate,Gentisate,4-Hydroxybenzoate,andα-Ketoglutarate by High-Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Anal Methodsuk,2015,7(16):6572-6578.
[12]孔燕凌.HPLC同时测定墨旱莲正丁醇有效部位含量分析[J].实验与检验医学,2017,35(4):475-478.
[13]Gliozzi G,Passeri S,Bortolani F,et al.Zeolite Catalysts for Phenol Benzoylation with Benzoic Acid:Exploring the Synthesis of Hydroxybenzophenones[J].Catalysts,2015,5(4):2223-2243.
[14]田莉,张炯怡,李静峰,等.HPLC法测定凉拌菜中苯甲酸、山梨酸和糖精钠的含量[J].中国调味品,2016,41(6):132-134.
[15]李向阳,高洁,屠万倩,等.RP-HPLC法测定逍遥丸(水丸)中芍药苷、苯甲酸和苯甲酰基总苷[J].中成药,2015,37(8):1722-1727.