摘要
目的对劲骨胶囊功效成分进行鉴别并对其主要的功效成分盐酸氨基葡萄糖的含量进行测定。方法采用化学反应法、薄层色谱法(thin-layer chromatography,TLC)及高效液相色谱法(high performance liquid chromatography,HPLC)鉴别功效成分及测定盐酸氨基葡萄糖含量。结果样品和盐酸氨基葡萄糖对照品与碱性酒石酸铜试液反应生成红色Cu2O沉淀,与硝酸银试液反应生成白色絮状AgCl沉淀,与茚三酮试液反应生成蓝紫色溶液,在薄层色谱相应位置上生成深红色斑点。样品和芍药苷对照品在薄层色谱相应位置上生成蓝紫色斑点。样品和碳酸钙对照品与稀盐酸试液反应产生CO2气体,与草酸铵试液反应生成白色CaC204沉淀。样品和维生素K1对照品及样品和维生素D3对照品高效液相色谱峰保留时间一致。所有阴性样品都无上述反应。通过高效液相色谱法测定样品中盐酸氨基葡萄糖含量,线性范围为96~1200μg/mL,相关系数为0.9999,方法检测限1.2μg/mL,精密度为0.72%,回收率为99.78%~100.40%。对连续3批样品盐酸氨基葡萄糖的含量进行测定,含量分别为64.94 g/100 g、64.25 g/100 g及65.12 g/100 g,相对标准偏差为0.48%。结论这种鉴别和含量测定方法专属性强、重现性好、灵敏度高,可管控产品质量,适合应用于劲骨胶囊功效成分鉴别及盐酸氨基葡萄糖含量测定工作中。
Objective To identify the effective components and determine the content of glucosamine hydrochloride in Jingu capsule.Methods Chemical reaction,thin layer chromatography(TLC)and high performance liquid chromatography(HPLC)were used for the effective components identification and determination of glucosamine hydrochloride content.Results Red Cu20 precipitate was formed by the reaction of sample and glucosamine hydrochloride with copper tartrate test solution,white flocculent AgCl precipitate was formed by the reaction with silver nitrate test solution,blue purple solution was formed by the reaction with ninhydrin test solution,and dark red spots were formed at corresponding positions of TLC.The sample and paeoniflorin reference substance generated blue-purple spots on the corresponding positions of TLC.The sample and calcium carbonate reference reacted with dilute hydrochloric acid test solution to generate CO2 gas and reacted with ammonium oxalate test solution to generate white CaC2 O4 precipitate.The retention time of HPLC peaks of the sample and vitamin K1 reference was the same as the sample and vitamin D3 reference.None of the negative samples had the above reaction.At the same time,the content of glucosamine hydrochloride in the sample was determined by HPLC.The linear relation was good with the linear coefficient r20.9999 in the linear range of 96~1200μg/mL.The limit of detection was 1.2μg/mL,the relative standard deviation(RSD)was 0.72%,and the recovery rates were 99.78%~100.40%.The glucosamine hydrochloride content of 3 consecutive batches of samples was determined and the results were 64.94 g/100 g,64.25 g/100 g and 65.12 g/100 g,respectively,with the RSD 0.48%.Conclusion These methods of identification and content determination have strong specificity,good reproducibility and high sensitivity,and could be used to control the product quality,which is suitable for the identification of effective components and determination of glucosamine hydrochloride content in Jingu capsule.
作者
张连龙
刁春霞
周华生
成恒嵩
任会娜
高伟
ZHANG Lian-Long;DIAO Chun-Xia;ZHOU Hua-Sheng;CHENG Heng-Song;REN Hui-Na;GAO Wei(Wuxi Giant Pharmaceutical Co.,Ltd,Wuxi 214091,China)
出处
《食品安全质量检测学报》
CAS
2020年第4期1271-1280,共10页
Journal of Food Safety and Quality
关键词
劲骨胶囊
保健食品
功效成分
盐酸氨基葡萄糖
鉴别
含量测定
Jingu capsule
health food
effective components
glucosamine hydrochloride
identification
content determination
