口腔溃疡系列制剂中冰片的定量检测和挥发性成分分析
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摘要
目的建立口腔溃疡系列制剂(片剂和散剂)中冰片的含量测定方法,同时分析制剂中的挥发性成分。方法采用气相色谱法测定制剂中的龙脑和异龙脑的含量,采用气相-质谱联用仪和顶空进样器分析制剂中的挥发性成分。结果异龙脑进样量线性范围为0.011 1～1.418 0μg,线性回归方程为Y=1.967 X+0.002,r=1.000(n=8),平均回收率为100.69%,RSD为3.42%(n=6);龙脑进样量线性范围为0.017 2～2.202 0μg,线性回归方程为Y=1.992 X+0.004,r=1.000(n=8),平均回收率为102.28%,RSD为3.01%(n=6)。制剂中主要成分为龙脑和异龙脑,部分样品含有薄荷醇(相对含量14.62%)和胡薄荷酮(相对含量6.22%)。结论该含量测定方法科学、简便、专属性较强,可有效控制制剂质量。个别样品中检出薄荷挥发油或提取物的色谱峰。
Objective To establish the content determination method of borneol in series preparations for treating oral ulcer,and to analyze the volatile constituents in the preparations. Methods GC method was used to determine the content of borneol and isoborneol in the preparations. The volatile constituents in the preparations were analyzed by GC-MS combined with headspace sampler. Results The isoborneol showed a good linear relationship in the rang of 0. 011 1-1. 418 0 μg, the linear regression equation was Y = 1. 967 X +0. 002, r = 1. 000( n = 8),the average recovery was 100. 69%,and the RSD was 3. 42%( n = 6). The borneol showed a good linear relationship in the rang of 0. 017 2-2. 202 0 μg, the linear regression equation was Y = 1. 992 X + 0. 004, r = 1. 000( n = 8), the average recovery was 102. 28%, and the RSD was 3. 01%( n = 6). The main constituents in the preparations were borneol and isoborneol, and some samples contained menthol( the relative amount was 14. 62%) and pulegone( the relative amount was 6. 22%). Conclusion The method is scientific, simple and specific, which can effectively control the quality of the preparations. The chromatographic peaks of volatile oil or extract of Mentha haplocalyx were detected in some samples.
Objective To establish the content determination method of borneol in series preparations for treating oral ulcer,and to analyze the volatile constituents in the preparations. Methods GC method was used to determine the content of borneol and isoborneol in the preparations. The volatile constituents in the preparations were analyzed by GC-MS combined with headspace sampler. Results The isoborneol showed a good linear relationship in the rang of 0. 011 1-1. 418 0 μg, the linear regression equation was Y = 1. 967 X +0. 002, r = 1. 000( n = 8),the average recovery was 100. 69%,and the RSD was 3. 42%( n = 6). The borneol showed a good linear relationship in the rang of 0. 017 2-2. 202 0 μg, the linear regression equation was Y = 1. 992 X + 0. 004, r = 1. 000( n = 8), the average recovery was 102. 28%, and the RSD was 3. 01%( n = 6). The main constituents in the preparations were borneol and isoborneol, and some samples contained menthol( the relative amount was 14. 62%) and pulegone( the relative amount was 6. 22%). Conclusion The method is scientific, simple and specific, which can effectively control the quality of the preparations. The chromatographic peaks of volatile oil or extract of Mentha haplocalyx were detected in some samples.
引文
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[10]孙亚栋,阿布力米提·阿布都卡德尔.薄荷叶挥发油成分的GC-MS分析[J].新疆大学学报(自然科学版),2017,34(1):61-63.
[11]靳有才,庆易薇,郭珍.青海野生薄荷挥发油成分GC-MS分析[J].中国实验方剂学杂志,2013,19(23):143-146.
[12]阎博,吴芳,刘海静,等.陕西野生薄荷挥发油化学成分的气相色谱-质谱分析[J].中国药业,2015,24(8):12-14.
[13]魏兴国,董岩,高朝明.春、秋季德州野生薄荷挥发油化学成分比较[J].江苏中医药,2006,27(2):48-50.
[2]付丽芳,刘金发,蔡铃英.口腔溃疡散中冰片的薄层色谱鉴别[J].光明中医,2008,23(12):1909.
[3]闫玮,张楠,刘建利.HPLC测定口腔溃疡散中色胺酮、靛蓝、靛玉红的含量[J].中成药,2009,31(5):743-745.
[4]闫占社,郭瑞,黄飙.口腔溃疡含片中青黛的薄层色谱鉴别方法研究[J].中国现代药物应用,2011,5(17):75-76.
[5]蔡长虹,迟强.HPLC法测定口腔溃疡含片中胸腺五肽的含量[J].医学研究杂志,2011,40(12):132-134.
[6]尤立华,杨秉呼,叶萌,等.气相色谱法同时测定大活络胶囊多组分含量[J].中国药业,2014,23(19):38-40.
[7]李彦超,李宜鲜,姚令文,等.GC法同时测定通络祛痛膏中樟脑、薄荷脑和冰片的含量[J].药物分析杂志,2012,32(4):672-675.
[8]姜家书,谢其亮,李敦明,等.气相色谱法测定通络祛痛膏中樟脑、薄荷脑和冰片含量[J].中国药业,2014,23(7):31-32.
[9]韩海红.气相色谱法测定珍珠明目滴眼液中龙脑含量[J].中国药业,2007,16(14):37.
[10]孙亚栋,阿布力米提·阿布都卡德尔.薄荷叶挥发油成分的GC-MS分析[J].新疆大学学报(自然科学版),2017,34(1):61-63.
[11]靳有才,庆易薇,郭珍.青海野生薄荷挥发油成分GC-MS分析[J].中国实验方剂学杂志,2013,19(23):143-146.
[12]阎博,吴芳,刘海静,等.陕西野生薄荷挥发油化学成分的气相色谱-质谱分析[J].中国药业,2015,24(8):12-14.
[13]魏兴国,董岩,高朝明.春、秋季德州野生薄荷挥发油化学成分比较[J].江苏中医药,2006,27(2):48-50.