麦角菌发酵物中 a麦角隐亭的RP-HPLC 测定方法

朱平;赵鸿莲;朱慧欣;王全;何惠霞

中国药学杂志 ›› 2000, Vol. 35 ›› Issue (04) : 260-262.

中国药学杂志 ›› 2000, Vol. 35 ›› Issue (04) : 260-262.
药品检验

麦角菌发酵物中 a麦角隐亭的RP-HPLC 测定方法

  • 朱平;赵鸿莲;朱慧欣;王全;何惠霞
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RP-HPLC assay for the determination of α-ergocryptine in the ergot fermentation products

  • Zhu Ping
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摘要

目的:建立麦角菌发酵产物a麦角隐亭的RP-HPLC定量测定方法,对在一定条件下a麦角隐亭发酵生产的峰值进行初步探索。方法:色谱柱(250 mm×4.6 mm,填料:YWG-C,10μm);流动相为甲醇-磷酸盐缓冲液(pH7.0)-乙酸乙酯(75:25:1);流速为1.0 ml·min;检测波长为312 nm。建立回归方程,进行方法精密度测定和加样回收率试验。结果:回归方程A=19058.54M+1352.66,r=0.9997,在0.6375~6.4375μg范围内线性关系良好;日内和日间相对标准偏差(RSD)分别为1.15%和0.44%;标准品浓度为122,244和488μg·ml时加样回收率分别为108.48%,105.15%,109.53%。用该方法测得a麦角隐亭发酵生产的峰值一般在发酵的第15~17d。结论:该方法在定量测定麦角菌发酵产物a麦角隐亭方面灵敏、准确。

Abstract

OBJECTIVE: To develop a reversed phase HPLC method for the quantitative determination of the ergot fermentation product α-ergocryptine and to determine the peak value of α-ergocryptine yielded during the fermentation. METHODS: A YWG-C18column (250 mm×4.6 mm ID,particle size,10 μm) was used;the mobile phase was MeOHphosphate buffer (pH7.0)EtOAc (75∶25∶1) with a flow rate of 1.0 ml·min-1and detected at 312 nm.A regression equation was set up,the precision of the method and the recovery rates were measured. RESULTS: Regression equation was A=19058.54M+1352.66,r=0.9997,over the range of 0.6375~6.4375 μg;the RSD for the intra day and inter day was 1.15%,0.44%,respectively;the mean recoveries were 108.48%,105.15% and 109.53% versus the added authentic sample at the concentrations of 122,244 and 488 μg·ml-1,respectively.The peak value appeared between day 15 to day 17 under the given condition. CONCLUSION: The method is sensitive and reproducible for the quantitative determination of the ergot fermentation product α-ergocryptine.

关键词

A-麦角隐亭 / 反相高效液相色语法 / 定童测定

Key words

α-ergocryptine / RP-HPLC / quantitative determination

引用本文

导出引用
朱平;赵鸿莲;朱慧欣;王全;何惠霞. 麦角菌发酵物中 a麦角隐亭的RP-HPLC 测定方法[J]. 中国药学杂志, 2000, 35(04): 260-262
Zhu Ping . RP-HPLC assay for the determination of α-ergocryptine in the ergot fermentation products[J]. Chinese Pharmaceutical Journal, 2000, 35(04): 260-262

参考文献

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