丁香油滴丸的制备工艺优化(1)
摘 要 目的：建立测定丁香油滴丸中丁香酚含量的方法，并对其制备工艺进行优化。方法：采用紫外-可见分光光度法测定丁香油滴丸中丁香酚的含量。在单因素试验基础上，以药物质量占总质量的百分比、药液温度、冷凝液下落距离、药液滴距为因素，以滴丸圆整度、硬度、质量差异及综合得分为指标，采用L9(34)正交设计试验对制备工艺进行优化，并进行验证试验和滴丸质量考察。结果：丁香酚质量浓度线性范围为15.15～45.45 μg/mL(r=0.999 6);精密度、稳定性、重复性试验的RSD均小于1%;加样回收率为97.41%～100.59%(RSD=1.35%，n=6)。最优制备工艺为药物质量占总质量的百分比为5%，药液温度为80 ℃，冷凝液下落距离为13 cm，药液滴距为6 cm。在此条件下，所得丁香油滴丸外观完整光洁，硬度适宜，圆整度较好;丁香酚平均含量为4.073%(RSD=0.35%，n=6)。结论：所建含量测定方法操作简单、方便，可用于测定丁香油滴丸中丁香酚的含量;优化所得制备工艺稳定、可行。
ABSTRACT OBJECTIVE： To establish the method for content determination of eugenol in Syzygium aromaticum oil dropping pills， and to optimize the preparation technology. METHODS： The content of eugenol in S. aromaticum oil dropping pills was determined by UV spectrophotometry. Based on single factor test， using the percentage of drugs in total amount， liquid temperature， falling distance of condensate， liquid drop distance as factors， taking the roundness， weight and hardness difference and comprehensive score as factors， L9(34) orthogonal design test was adopted to optimize the preparation process. RESULTS： The linear range of eugenol was 15.15-45.45 μg/mL(r=0.999 6); RSDs of precision， stability and reproducibility tests were all lower than 1%; the recoveries were 97.41%-100.59%(RSD=1.35%， n=6). The optimal preparation technology included that the percentage of drugs in total amount was 5%; liquid temperature was 80 ℃; falling distance of condensate was 13 cm; liquid drop distance was 6 cm. The dropping pills had smooth appearance， good roundness and moderate hardness; the average content of engenol was 4.073%(RSD=0.35%，n=6). CONCLUSIONS： The established method is simple， and can be used for the content determination of eugenol in S. aromaticum oil dropping pills. The optimal preparation technology is stable and feasible.
KEYWORDS Syzygium aromaticum oil dropping pills; Eugenol; UV spectrophotometry; Content determination; Preparation technology; Optimization; Orthogonal design
丁香(Eugenia caryophyllata Thunb.)為桃金娘科植物丁香树的干燥花蕾。丁香油是丁香花蕾经水蒸气蒸馏得到的挥发油，其主要活性成分为丁香酚，含量约为80%～87%，具有抑菌[1]、抗氧化[2-3]、抗缺氧[4-5]、抗血栓[6]、抗凝、抗血小板聚集[7]、疏通血管、镇痛[8]等作用。虽然已有文献报道了丁香油膜剂、栓剂等非口服局部给药制剂[8-9]，但这些剂型在使用方式上存在诸多不便。而将丁香油制成经口服给药的滴丸可达到使用方便、快速起效的目的，具有较好的开发应用前景[10]，而且目前也尚无关于丁香油滴丸研究的报道。为此，本研究采用紫外-分光光度法(UV)测定丁香油滴丸中丁香酚的含量，采用正交设计对该滴丸制备工艺进行优化，旨在为其药理、药效研究提供依据，也为开发丁香油新制剂提供参考。
1 材料
1.1 仪器
752N型UV计(上海仪电分析仪器有限公司);SIM-F140AY65-PC型制冰机[松下冷链(大连)有限公司];RO-2236P型Tankpro纯水机(浙江铭泉水暖设备有限公司);eppendorf 1 000 μL移液枪(德国艾文德集团公司);HWS-12型电热恒温水浴锅(上海一恒科学仪器有限公司);YPD-30A型片剂硬度仪、CJY-300D型片剂脆碎度测定仪(上海黄海药检仪器有限公司);AL204型万分之一电子天平[梅特勒-托利多仪器(上海)有限公司]。, http://www.100md.com(杜卓 余小姚 邝翠琼 莫玉芳 周宝珠 刘露 李海仪 郭嘉亮)
ABSTRACT OBJECTIVE： To establish the method for content determination of eugenol in Syzygium aromaticum oil dropping pills， and to optimize the preparation technology. METHODS： The content of eugenol in S. aromaticum oil dropping pills was determined by UV spectrophotometry. Based on single factor test， using the percentage of drugs in total amount， liquid temperature， falling distance of condensate， liquid drop distance as factors， taking the roundness， weight and hardness difference and comprehensive score as factors， L9(34) orthogonal design test was adopted to optimize the preparation process. RESULTS： The linear range of eugenol was 15.15-45.45 μg/mL(r=0.999 6); RSDs of precision， stability and reproducibility tests were all lower than 1%; the recoveries were 97.41%-100.59%(RSD=1.35%， n=6). The optimal preparation technology included that the percentage of drugs in total amount was 5%; liquid temperature was 80 ℃; falling distance of condensate was 13 cm; liquid drop distance was 6 cm. The dropping pills had smooth appearance， good roundness and moderate hardness; the average content of engenol was 4.073%(RSD=0.35%，n=6). CONCLUSIONS： The established method is simple， and can be used for the content determination of eugenol in S. aromaticum oil dropping pills. The optimal preparation technology is stable and feasible.
KEYWORDS Syzygium aromaticum oil dropping pills; Eugenol; UV spectrophotometry; Content determination; Preparation technology; Optimization; Orthogonal design
丁香(Eugenia caryophyllata Thunb.)為桃金娘科植物丁香树的干燥花蕾。丁香油是丁香花蕾经水蒸气蒸馏得到的挥发油，其主要活性成分为丁香酚，含量约为80%～87%，具有抑菌[1]、抗氧化[2-3]、抗缺氧[4-5]、抗血栓[6]、抗凝、抗血小板聚集[7]、疏通血管、镇痛[8]等作用。虽然已有文献报道了丁香油膜剂、栓剂等非口服局部给药制剂[8-9]，但这些剂型在使用方式上存在诸多不便。而将丁香油制成经口服给药的滴丸可达到使用方便、快速起效的目的，具有较好的开发应用前景[10]，而且目前也尚无关于丁香油滴丸研究的报道。为此，本研究采用紫外-分光光度法(UV)测定丁香油滴丸中丁香酚的含量，采用正交设计对该滴丸制备工艺进行优化，旨在为其药理、药效研究提供依据，也为开发丁香油新制剂提供参考。
1 材料
1.1 仪器
752N型UV计(上海仪电分析仪器有限公司);SIM-F140AY65-PC型制冰机[松下冷链(大连)有限公司];RO-2236P型Tankpro纯水机(浙江铭泉水暖设备有限公司);eppendorf 1 000 μL移液枪(德国艾文德集团公司);HWS-12型电热恒温水浴锅(上海一恒科学仪器有限公司);YPD-30A型片剂硬度仪、CJY-300D型片剂脆碎度测定仪(上海黄海药检仪器有限公司);AL204型万分之一电子天平[梅特勒-托利多仪器(上海)有限公司]。, http://www.100md.com(杜卓 余小姚 邝翠琼 莫玉芳 周宝珠 刘露 李海仪 郭嘉亮)
参见：首页 > 中医药 > 中药专业 > 中草药汇编 > 中药大典 > 花类 > 丁香