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目的:了解低温配制工艺对虎杖膏中总二苯乙烯和总蒽醌含量的影响。方法:采用将虎杖粉加入80 ℃麻油中的低温配制工艺制备虎杖膏;以虎杖苷为对照品,采用一阶导数光谱法在343 nm和345 nm波长处测定虎杖膏中总二苯乙烯的含量;以大黄素为对照品,采用分光光度法在437 nm波长处测定虎杖膏中总蒽醌的含量。计算虎杖膏制备过程中总二苯乙烯和总蒽醌的转移率。结果:虎杖苷、大黄素检测质量浓度线性范围分别为4.24~14.84 μg/mL(r=0.999 9)和3.96~13.86 μg/mL(r=0.999 5);精密度、稳定性(6 h)、重复性试验的RSD均<3%(n=6或n=7);平均回收率分别为99.43%、98.70%,RSD分别为0.94%、0.91%(n=6);测得3批虎杖粉及制得的虎杖膏所含虎杖粉中总二苯乙烯(以虎杖苷计)的平均含量分别为(29.444±0.445)、(29.518±0.437)、(28.323±0.609)和(26.558±0.227)、(28.045±0.303)、(25.290±0.781) mg/g,总蒽醌(以大黄素计)的平均含量分别为(20.557±0.257)、(19.520±0.292)、(18.795±0.444)和(18.438±0.240)、(18.621±0.017)、(16.808±0.076) mg/g,3批虎杖加入80 ℃麻油调配成软膏后,总二苯乙烯和总蒽醌转移率分别为(90.22±2.13)%、(95.01±0.38)%、(89.28±0.84)%和(89.71±2.29)%、(95.41±1.52)%、(89.46±2.52)%。结论:采用较低油温(80 ℃)中加入虎杖粉进行调配虎杖膏,总二苯乙烯和总蒽醌的转移率均在89%以上,表明该低温配制工艺能较好地避免热敏性成分受到破坏,具有合理性。
OBJECTIVE: To investigate the effects of low-temperature preparation technology on the contents of total stilbenes and total anthraquinone in Polygonum cuspidatum ointment. METHODS: Using low-temperature preparation technology by adding P. cuspidatum powder into the sesame oil at lower oil temperature (80 ℃) to prepare Polygonum cuspidatum ointment. The content of total stilbene in P. cuspidatum ointment was determined by first-order derivative spectrophotometry at 343 nm and 345 nm using polydatin as control. The content of total anthraquinone in P. cuspidatum ointment was determined by spectrophotometry at 437 nm using emodin as control. The transfer rate of total stilbene and total anthraquinone in the preparation process of P. cuspidatum ointment were calculated. RESULTS: The linear ranges of polydatin and emodin were 4.24-14.84 μg/mL (r=0.999 9) and 3.96-13.86 μg/mL (r=0.999 5), respectively. RSDs of precision, stability (6 h) and repeatability tests were all less than 3% (n=6 or n=7). The average recoveries were 99.43% and 98.70%, and RSD were 0.94% and 0.91% (n=6), respectively. The average contents of total stilbene (by polydatin) in 3 batches of P. cuspidatum and P. cuspidatum ointment were (29.444±0.445), (29.518±0.437), (28.323±0.609) and (26.558±0.227), (28.045±0.303), (25.290±0.781) mg/g, respectively. The average contents of total anthraquinone (by emodin) were (20.557±0.257), (19.520±0.292), (18.795±0.444), (18.438±0.240), (18.621±0.017), (16.808±0.076) mg/g, respectively. The transfer rates of total stilbene and total anthraquinone were (90.22±2.13)%, (95.01±0.38)%, (89.28±0.84)% and (89.71±2.29)%, (95.41±1.52)% and (89.46±2.52)% after 3 batches of P. cuspidatum were added to 80 ℃ sesame oil to form ointment. CONCLUSIONS: The transfer rates of total stilbene and total anthraquinone are all over than 89% in add P. cuspidatum powder into the sesame oil at lower oil temperature (80 ℃), which indicates that it is rational to using low temperature preparation technology, and it can avoid the destruction of heat sensitive component.
虎杖膏麻油低温配制转移率分光光度法一阶导数光谱法总二苯乙烯总蒽醌虎杖苷大黄素
Polygonum cuspidatum ointmentSesame oilLow-temperature preparation technologyTransfer rateSpectrophotometryFirst derivative spectrophotometryTotal stilbeneTotal anthraquinonePolydatinEmodin
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