首页> 美国卫生研究院文献>Journal of Zhejiang University. Science. B >Identification and determination of major constituents in a traditional Chinese medicine compound recipe Xiongdankaiming tablet using HPLC-PDA/ESI-MSn and HPLC-UV/ELSD
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Identification and determination of major constituents in a traditional Chinese medicine compound recipe Xiongdankaiming tablet using HPLC-PDA/ESI-MSn and HPLC-UV/ELSD

机译:HPLC-PDA / ESI-MSn和HPLC-UV / ELSD鉴别和测定中药复方熊胆开明片中的主要成分

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摘要

Xiongdankaiming tablet (XDKMT), a well-known compound in traditional Chinese medicine, is widely used for the treatment of acute iridocyclitis and primary open-angle glaucoma. In this paper, accurate and reliable methods were developed for the identification of 20 constituents using high-performance liquid chromatography with photo-diode array and electron spray ionization-mass spectrometry (HPLC-PDA/ESI-MSn), and determination of nine of the constituents (chlorogenic acid, gentiopicroside, isochlorogenic acid B, diosmetin-7-O-β-D-glucopyranoside, apigenin, diosmetin, tauroursodeoxycholic acid, acacetin, and taurochenodeoxycholic acid) was developed using HPLC with ultraviolet absorption detector and evaporative light scattering detector (HPLC-UV/ELSD) for the first time. The best results were obtained on a Zorbax SB-C18 column with gradient elution using water (0.1% formic acid) (A) and methanol (0.1% formic acid) (B) at a flow rate of 0.7 ml/min. Tauroursodeoxycholic acid and taurochenodeoxycholic acid, owing to their low UV absorption, were detected by ELSD. The other seven compounds were analyzed by HPLC-UV with variable wavelengths. The calibration curves of all nine constituents showed good linear regression (R 2>0.9996) within the linearity ranges. The limits of detection and quantification were in the ranges of 0.0460–9.90 μg/ml and 0.115–24.8 μg/ml, respectively. The accuracy, in terms of recovery, varied from 95.3% to 104.9% with relative standard deviations (RSDs) less than 4.4%. Precision (with the intra- and inter-day variations less than 4.4%) was also suitable for its intended use. The developed method was successfully applied for the analysis of major components in XDKMT, which provides an appropriate method for the quality control of XDKMT.
机译:雄丹开明片(XDKMT)是中药中的知名化合物,被广泛用于治疗急性虹膜睫状体炎和原发性开角型青光眼。本文开发了使用光电二极管阵列和电子喷雾电离质谱(HPLC-PDA / ESI-MS n )的高效液相色谱法鉴定20种成分的准确可靠的方法),并使用HPLC和紫外光谱法开发了9种成分的测定方法(绿原酸,龙胆苦苷,异绿原酸B,薯-7皂素-7-O-β-D-吡喃葡萄糖苷,芹菜素,薯os皂素,牛磺去氧胆酸,阿沙西汀和牛磺去氧胆酸)吸收检测器和蒸发光散射检测器(HPLC-UV / ELSD)首次出现。在Zorbax SB-C18色谱柱上,使用水(0.1%甲酸)(A)和甲醇(0.1%甲酸)(B)以0.7 ml / min的流速进行梯度洗脱,可获得最佳结果。牛磺去氧胆酸和牛磺去氧胆酸由于其低紫外线吸收而被ELSD检测到。通过HPLC-UV以可变波长分析其他七个化合物。所有九种成分的校准曲线在线性范围内均表现出良好的线性回归(R 2

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