摘要
目的建立快速测定转化熊胆粉中牛磺熊去氧胆酸(TUDCA)和牛磺鹅去氧胆酸(TCDCA)含量的高效液相色谱-蒸发光散射器检测法。方法采用涡旋提取法制备样品。色谱柱为Agilent Poroshell 120 SB-C_(18)柱(30 mm×4.6 mm,2.7μm),流动相为5 mmol/L乙酸铵水溶液-乙腈(梯度洗脱),流速为1.0 mL/min,柱温为40℃,进样量为5μL,蒸发器温度为120℃,雾化器温度为60℃,气体流速为1.60 L/min。结果该方法可在6 min内完成样品的提取和分析。TUDCA和TCDCA的质量浓度分别在52.71~527.10μg/mL、49.80~497.97μg/mL范围内与峰面积线性关系良好(r≥0.9998);检测限分别为7.91,3.73μg/mL,定量限分别为15.81,7.47μg/mL;精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率分别为97.31%和101.34%,RSD分别为1.64%和1.20%(n=6)。10批样品中TUDCA和TCDCA的平均含量分别为36.07%和21.76%。结论该方法操作简便、快速灵敏、重复性好、专属性强、结果准确,可快速、高效地测定转化熊胆粉中TUDCA和TCDCA的含量。
Objective To establish a high-performance liquid chromatography(HPLC)-evaporative light scattering detector(ELSD)method for rapid determination of tauroursodeoxycholic acid(TUDCA)and taurochenodeoxycholic acid(TCDCA)in transformed bear bile powder.Methods The sample was prepared by the vortex extraction method.The chromatographic column was Agilent Poroshell 120 SB-C_(18) column(30 mm×4.6 mm,2.7μm),the mobile phase was 5 mmol/L ammonium acetate aqueous solution-acetonitrile(gradient elution),the flow rate was 1.0 mL/min,the column temperature was 40℃,the injection volume was 5μL,the temperature of evaporator was 120℃,the temperature of atomizer was 60℃,and the flow rate of gas was 1.60 L/min.Results This method could complete sample extraction and analysis within 6 min.The linear ranges of TUDCA and TCDCA were 52.71-527.10μg/mL and 49.80-497.97μg/mL(r≥0.9998),respectively.The limits of detection were 7.91μg/mL and 3.73μg/mL,respectively.The limits of quantification were 15.81μg/mL and 7.47μg/mL,respectively.The RSDs of precision,stability,and repeatability test results were all lower than 2.0%.The average recoveries of TUDCA and TCDCA were 97.31%and 101.34%,with RSDs of 1.64%and 1.20%(n=6),respectively.The average contents of TUDCA and TCDCA in 10 batches of samples were 36.07%and 21.76%,respectively.Conclusion This method is simple,fast and sensitive,with good repeatability,strong specificity,and accurate results,which can quickly and efficiently determine the content of TUDCA and TCDCA in transformed bear bile powder.
作者
何焯斌
黄琦
王枫
吴齐龙
梅全喜
钱正明
HE Zhuobin;HUANG Qi;WANG Feng;WU Qilong;MEI Quanxi;QIAN Zhengming(Dongguan HEC Cordyceps R&D Co.,Ltd.,Dongguan,Guangdong,China 523850;Linzhi HEC PHARM R&D CO.,Ltd.,Linzhi,Xizang,China 860001;Chongqing Kinbear Biotechnology Co.,Ltd.,Chongqing,China 400799;Shenzhen Baoan Traditional Chinese Medicine Hospital,Shenzhen,Guangdong,China 518000)
出处
《中国药业》
2025年第13期89-92,共4页
China Pharmaceuticals
基金
广东省药品监督管理局科技创新项目[2021ZDB05]。
