小儿化毒系列制剂中冰片投料质量分析
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摘要
目的:建立检测小儿化毒系列制剂中冰片的气相色谱法,并对冰片的投料质量进行研究,以完善和统一小儿化毒中冰片的质量标准。方法:采用气相色谱法。色谱柱为HP-INNOWax毛细管色谱柱,程序升温,检测器为氢火焰离子化检测器,检测器温度为240℃,载气为氮气,流速为2.0 m L/min,分流比为30∶1,进样量为1.0μL。结果:龙脑进样量在0.117 5～1.880μg范围内、异龙脑进样量在0.098 48～1.575 6μg范围内、冰片进样量在0.112 8～1.80 5μg范围内,峰面积积分值与进样量呈良好的线性关系(r=0.999 8、0.999 7、0.999 8);精密度、稳定性、重复性试验的RSD<3.0%;龙脑、异龙脑加样回收率分别为103.52%、97.98%。个别批次样品中樟脑检出含量接近检测限。结论:该方法简便、准确,适用于全面控制该制剂中冰片的投料质量。
Objective: To establish a gas chromatographic method for detection of Borneol in Xiao'erhuadu Series Preparations,and to study the quality of borneo to improve and unify the quality standards of borneo in that. Methods: GC method was adopted. The determination was performed on HP-INNOWax capillary column at the rate of 2.0 mL/min using nitrogen gas as carrier and FID as the detector by temperature programming. The temperature of detector was set at 240℃. Carries gas was nitrogen. The split ratio was 30:1. The sample size was 1.0 μL. Results: borneol sample quantity is within the scope of 0.117 5-1.880μg,isoborneol sample quantity is within the scope of 0.098 48-1.575 6μg,borneol sample quantity in range of 0.112 8-1.805μg,the peak area of integral value and quantity of sample had good linear relationship( r = 0.999 8,0.999 7,0.999 8),RSDs of precision,stability and reproducibility tests were all lower than 3.0%. The recovery rate of borneol and isoborneol is 103.52% and 97.98%. The detection of camphor in individual batches is close to the detection limit. Conclusion: The method is simple and accurate,is suitable for comprehensively controlling the feeding quality of Borneol in the preparation.
Objective: To establish a gas chromatographic method for detection of Borneol in Xiao'erhuadu Series Preparations,and to study the quality of borneo to improve and unify the quality standards of borneo in that. Methods: GC method was adopted. The determination was performed on HP-INNOWax capillary column at the rate of 2.0 mL/min using nitrogen gas as carrier and FID as the detector by temperature programming. The temperature of detector was set at 240℃. Carries gas was nitrogen. The split ratio was 30:1. The sample size was 1.0 μL. Results: borneol sample quantity is within the scope of 0.117 5-1.880μg,isoborneol sample quantity is within the scope of 0.098 48-1.575 6μg,borneol sample quantity in range of 0.112 8-1.805μg,the peak area of integral value and quantity of sample had good linear relationship( r = 0.999 8,0.999 7,0.999 8),RSDs of precision,stability and reproducibility tests were all lower than 3.0%. The recovery rate of borneol and isoborneol is 103.52% and 97.98%. The detection of camphor in individual batches is close to the detection limit. Conclusion: The method is simple and accurate,is suitable for comprehensively controlling the feeding quality of Borneol in the preparation.
引文
[1]国家药典委员会.中华人民共和国药典:一部[S].北京:中国医药科技出版社,2015:630.
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[3]姜梦丽,范哲贤,杨真真,等.气相色谱法测定芳冰鼻吸剂中芳樟醇、冰片、薄荷醇的含量[J].福建中医药大学学报,2014,24(5):34-36.
[4]曾小平,陈新国,黄俊忠.GC法测定克痒敏醑中薄荷脑、冰片和水杨酸甲酯的含量[J].中药新药与临床药理,2014,25(01):74-76.
[5]罗忠生,蒋志茵,罗汉宇,等.GC法测定天然冰片中的d-龙脑和樟脑[J].江西林业科技,2014,42(5):52-53.
[6]朱殿龙,梁云,孙楠,等.气相色谱法测定田七痛经胶囊中冰片的含量[J].中国医院用药评价与分析,2017,17(5):664-666.
[7]闵祺,王闯.气相色谱法同时测定苏合香丸中龙脑、丁香酚及麝香酮的含量[J].药物分析杂志,2018,38(02):359-363.
[2]吴芳,樊宝娟,乔蓉霞.气相色谱法鉴别小儿化毒胶囊中冰片、乳香和没药[J].安徽医药,2011,15(11):1356-1357.
[3]姜梦丽,范哲贤,杨真真,等.气相色谱法测定芳冰鼻吸剂中芳樟醇、冰片、薄荷醇的含量[J].福建中医药大学学报,2014,24(5):34-36.
[4]曾小平,陈新国,黄俊忠.GC法测定克痒敏醑中薄荷脑、冰片和水杨酸甲酯的含量[J].中药新药与临床药理,2014,25(01):74-76.
[5]罗忠生,蒋志茵,罗汉宇,等.GC法测定天然冰片中的d-龙脑和樟脑[J].江西林业科技,2014,42(5):52-53.
[6]朱殿龙,梁云,孙楠,等.气相色谱法测定田七痛经胶囊中冰片的含量[J].中国医院用药评价与分析,2017,17(5):664-666.
[7]闵祺,王闯.气相色谱法同时测定苏合香丸中龙脑、丁香酚及麝香酮的含量[J].药物分析杂志,2018,38(02):359-363.