HPLC-MS测定十味龙胆花颗粒中的龙胆苦苷和小檗碱  

HPLC-MS simultaneous determination of gentiopicrin and berberine in Shiwei Longdanhua granules

作　　者：许海棠[1] 黄丽涵[1] 曾永芳[1] 徐远金[1,2] 

机构地区：[1]广西大学糖业工程技术研究中心,南宁530004 [2]广西亚热带生物资源保护利用重点实验室,南宁530004

出　　处：《药物分析杂志》2008年第10期1641-1644,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立一种快速灵敏的同时测定十味龙胆花颗粒中的有效成分龙胆苦苷和小檗碱的HPLC-MS方法。方法:样品用50%甲醇溶液超声提取,采用Zorbax SB C_(18)(4.6 mm×250 mm,5 μm)色谱柱,以含0.2 mmol·L^(-1)醋酸钠的1%醋酸水溶液(A)-甲醇(B)为流动相进行梯度洗脱(0～10 min,33%B;19 min,60%B;19.01 min,80%B),流速0.8 mL·min^(-1);在ESI正离子模式下,采用选择性离子监测方法(0～14 min,m/z 379;14～22 min,m/z 336)。结果:龙胆苦苷、小檗碱的线性范围分别为0.030～30.0 μg·mL^(-1)(r=0.9992)和0.004～10.0 μg·mL^(-1)(r=0.9990),检出限分别为0.010 μg·mL^(-1)和0.0013 μg·mL^(-1),样品加样回收率为99.2%～103.3%,日内、日间精密度试验的RSD均低于5%。结论:方法快捷、准确,重复性好,可用于药品十味龙胆花颗粒的分析。Objective：To establish an HPLC - MS method for simultaneous determination of gentiopicrin and ber- berine in Shiwei Longdanhua granules. Method：The sample were extracted with 50% methanol aqueous solution using ultrasound- assisted extraction. The HPLC separation was performed on Zorbax SB C18 （4. 6 mm × 250 mm,5 μm） column using water（A）, containing 0. 2 mmol · L^-1 sodium acetate and 1% acetic acid, and methanol（B） as mobile phase,with the gradient elution （0 - 10 rain,33% B;19 min,60% B;19.01 min,80%B） at a flow rate of 0. 8 mL · min^-1. The analytes were detected by ESI - MS under ion monitoring mode （0 - 14 min,m/z 379;14 - 22 min, m/z 336 ）. Results ： The linear ranges were 0. 030 - 30. 0 μg · mL^ -1 （ r = 0. 9992 ） and 0. 004 - 10 μg · mL^-1（r =0. 9990）,with detection limits of 0. 010μg· mL^-1 and 0. 0013 μg · mL^-1 for gentiopierin and berberine, respectively. The average recoveries ranged from 99.2% to 103.3 %. The relative standard deviations of intra - day and inter- day were less than 5%. Conclusion： The method is accurate, sensitive, rapid, and suitable for the quality control of gentiopicrin and berberine in Shiwei Longdanhua granules.

关 键 词：十味龙胆花颗粒 龙胆苦苷 小檗碱 高效液相色谱-质谱联用法 

分 类 号：R917[医药卫生—药物分析学]