高效液相色谱法测定地塞米松植入剂的有关物质
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摘要
目的建立高效液相色谱测定地塞米松植入剂有关物质的方法。方法采用天津兰博Kromasil-C18柱(250 mm×4.6mm,5μm),流动相为乙腈—水(28∶72,V/V),流速为2.0 m L·min-1,检测波长为240 nm,柱温:35℃。结果地塞米松与有关物质分离良好,辅料不干扰测定;地塞米松、倍他米松在0.1~10 mg·L-1范围内线性关系良好;倍他米松低、中、高3种浓度的加样平均回收率为:98.23%,RSD为:0.61%,地塞米松与倍他米松的定量限、检测限依次为:1.17、1.04、0.39、0.34μg·L-1。在室温下供试品溶液可稳定8 h。结论该方法操作简便准确、灵敏度高,适用于地塞米松植入剂有关物质检查。
Objective To establish an HPLC method for the determination of related substances of dexamethasone implants. Methods A Kromasil-C18column( 250 mm × 4. 6 mm,5 μm) was adopted with a mobile phase of a mixture of acethane-water( 28 ∶ 72) at a flow rate of 2. 0 m L·min- 1and UV detector wavelength at 240 nm. The column tempreture was 35 ℃. Results Dexamethasone and related substances could be baseline separated,and the excipients didn't interfere with the determination. The linear ranges of dexamethasone and betamethasone were both 0. 1 ~ 10 mg·L- 1. The average recoveries at low,middle and high concentration of betamethasone were all 98. 23%. RSD was 0. 61%. The LOQ,LOD of dexamethasone and betamethasone were 1. 17,1. 04,0. 39,and 0. 34 μg·L- 1respectively,The sample solution was steady within 8 h at room temperature. Conclusion This method is rapid,accurate and sensitive,which can be used for determination of the content and related substances of dexamethasone implants.
Objective To establish an HPLC method for the determination of related substances of dexamethasone implants. Methods A Kromasil-C18column( 250 mm × 4. 6 mm,5 μm) was adopted with a mobile phase of a mixture of acethane-water( 28 ∶ 72) at a flow rate of 2. 0 m L·min- 1and UV detector wavelength at 240 nm. The column tempreture was 35 ℃. Results Dexamethasone and related substances could be baseline separated,and the excipients didn't interfere with the determination. The linear ranges of dexamethasone and betamethasone were both 0. 1 ~ 10 mg·L- 1. The average recoveries at low,middle and high concentration of betamethasone were all 98. 23%. RSD was 0. 61%. The LOQ,LOD of dexamethasone and betamethasone were 1. 17,1. 04,0. 39,and 0. 34 μg·L- 1respectively,The sample solution was steady within 8 h at room temperature. Conclusion This method is rapid,accurate and sensitive,which can be used for determination of the content and related substances of dexamethasone implants.
引文
[1]任翠丽,尹情胜,俞敏,等.HPLC法测定地塞米松植入剂的含量[J].安徽医药,2013,17(8):1294-1295.
[2]刘干炎,王水华,刘永芳,等.地塞米松、盐酸氮芥、降纤酶联合治疗紫瘫性肾炎的疗效观察[J].中国医药指南,2012,10(26):202-203.
[3]高大明,翟爱国,刘永红,等.小剂量激素短疗程辅助治疗支原体肺炎临床观察[J].安徽医药,2010,14(6):713-714.
[4]李群.HPLC法测定醋酸地塞米松片有关物质[J].中国医药科学,2012,2(5):99-100.
[5]李洁.地塞米松磷酸钠注射液有关物质检查方法的探讨[J].中国药事,2013,27(4):416-419.
[6]孙超,张昊天,尹燕杰,等.地塞米松磷酸钠注射液有关物质检验方法分析[J].黑龙江医药,2013,126(3):392-393.
[7]王国兰,寇晋萍,王俊秋,等.反相HPLC法同时测定复方氧氟沙星滴眼液中氧氟沙星和地塞米松磷酸钠的含量及有关物质[J].中国药品标准,2010,11(3):195-198.
[8]方海燕.地塞米松磷酸钠注射液的质量分析[J].临床合理用药,2012,5(9):45.
[9]Zhang CL,Gao P,Yin WF,et al.Dexamethasone regulates differential expression of carboxylesterase 1 and carboxylesterase 2through activation of nuclear receptors[J].Huazhong Univ Sci Technol,2012,32(6):798-805.
[10]林琪珊,洪淑华,余良钟.复方醋酸地塞米松乳膏有关物质的测定及其杂质的确定[J].中国药房,2013,24(9):843-845.
[11]吴燕,张福成,徐荣,等.高效液相色谱法同时测定复方咽炎喷雾剂中3种药物含量[J].中国新药杂志,2012,21(3):324-326.
[12]Zhang RL,Bo T,Shen L,et al.Effect of dexamethasone on intelligence and hearing in preterm infants:a meta-analysis[J].Neural Regeneration Research,2014,9(6):637-645.
[13]左志辉,唐素芳.HPLC法测定倍他米松及其乳膏的含量及有关物质[J].药物分析杂志,2009,29(12):2162-2165.
[14]国家药典委员会.中国药典(二部)[S].北京:中国医药科技出版社,2010:249.
[2]刘干炎,王水华,刘永芳,等.地塞米松、盐酸氮芥、降纤酶联合治疗紫瘫性肾炎的疗效观察[J].中国医药指南,2012,10(26):202-203.
[3]高大明,翟爱国,刘永红,等.小剂量激素短疗程辅助治疗支原体肺炎临床观察[J].安徽医药,2010,14(6):713-714.
[4]李群.HPLC法测定醋酸地塞米松片有关物质[J].中国医药科学,2012,2(5):99-100.
[5]李洁.地塞米松磷酸钠注射液有关物质检查方法的探讨[J].中国药事,2013,27(4):416-419.
[6]孙超,张昊天,尹燕杰,等.地塞米松磷酸钠注射液有关物质检验方法分析[J].黑龙江医药,2013,126(3):392-393.
[7]王国兰,寇晋萍,王俊秋,等.反相HPLC法同时测定复方氧氟沙星滴眼液中氧氟沙星和地塞米松磷酸钠的含量及有关物质[J].中国药品标准,2010,11(3):195-198.
[8]方海燕.地塞米松磷酸钠注射液的质量分析[J].临床合理用药,2012,5(9):45.
[9]Zhang CL,Gao P,Yin WF,et al.Dexamethasone regulates differential expression of carboxylesterase 1 and carboxylesterase 2through activation of nuclear receptors[J].Huazhong Univ Sci Technol,2012,32(6):798-805.
[10]林琪珊,洪淑华,余良钟.复方醋酸地塞米松乳膏有关物质的测定及其杂质的确定[J].中国药房,2013,24(9):843-845.
[11]吴燕,张福成,徐荣,等.高效液相色谱法同时测定复方咽炎喷雾剂中3种药物含量[J].中国新药杂志,2012,21(3):324-326.
[12]Zhang RL,Bo T,Shen L,et al.Effect of dexamethasone on intelligence and hearing in preterm infants:a meta-analysis[J].Neural Regeneration Research,2014,9(6):637-645.
[13]左志辉,唐素芳.HPLC法测定倍他米松及其乳膏的含量及有关物质[J].药物分析杂志,2009,29(12):2162-2165.
[14]国家药典委员会.中国药典(二部)[S].北京:中国医药科技出版社,2010:249.