当归注射液中5-羟甲基呋喃甲醛的鉴定与含量测定  

Identification and Determination of 5-Hydroxymethylfurfural in Angelica Injection

作　　者：尹登科[1] 丁虹[1] 方世平[2] 喻昕[1] 

机构地区：[1]武汉大学药学院,武汉430072 [2]武汉大学中南医院,武汉430072

出　　处：《药物分析杂志》2005年第2期192-194,共3页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:鉴定当归注射液中5-羟甲基呋喃甲醛(5-Hydroxymethyl-furfural,HMF),以及建立该组分高效液相色谱含量检测的方法。方法:用醋酸乙酯萃取当归注射液,萃取相采用气相色谱/质谱联用仪检测,色谱柱:Alltech AT^(TM-5)(30 m×0.2mm×0.2 μm),载气为高纯氦气,流速1 mL·min^(-1),进样口温度220℃,柱温70℃,保持1 min,以10℃·min^(-1)的速率升温到200℃,保持1 min,再以20℃·min^(-1)升温到270℃,保持5 min;质谱检测总离子流。气相色谱保留时间为8.06 min的峰对应的质谱图经数据库分析可能是HMF。用对照品进行了气相色谱/质谱和高效液相色谱验证,高效液相色谱条件:采用Agilent Zorbax C_(18)色谱柱(150 mm ×2.1 mm×5μm),流动相:甲醇(B),1%冰醋酸(A),10%B-90%A→90%A-10%B(25 min)线性洗脱,流速:1 mL·min^(-1),检测波长:320 nm,柱温:30℃。并建立当归注射液中HMF含量的高效液相定量测定方法。结果:当归注射液中含有HMF,高效液相色谱法适用于当归注射液中HMF含量的检测。Objective: Identification and quantitation of 5-Hydroxymethyl-furfural (HMF) in Angelica injection. Methods: Ethyl acetate extract of Angelica injection was analyzed with GC/MS, the gas chromatographic conditions was advanced as follows: Alltech AT^(TM-5) (30 m×0.2 mm×0.2μm) column,high purity helium was used as carries gas with flow rate at 1 mL·min^(-1); Injector temperature: 220℃; Column temperature: 70℃ keeping 1 min,from 70 ℃ to 200℃ (10℃· min^(-1)) , keeping for 1 min, then from 200℃ to 270℃ (20℃· min^(-1)) keeping for 5 min; MS detected with total ion monitoring. The MS of retention time of 8.06 min on GC is matched with reference standard HMF. It was demonstrated that HMF existed in Angelica Infection through GC/MS and HPLC methods with standard HMF. The condition of HPLC as follows: Agilent Zorbax C_(18) column (150 mm×2.1 mm×5μm) ,the mobile phase: methanol(B) , 1% acetic acid (A) , 10% B-90% A→90% A-10% B (25 min) , flow rate: 1 mL·min^(-1),detective wave length:320nm,column temperature:30℃ and the HPLC method for quantitation of HMF was established. Result: Angelica injection contains HMF and the HPLC method for quantitation of HMF in Angelica Injection is effective.

关 键 词：当归注射液 5-羟甲基呋喃甲醛 鉴定 含量 测定 中药 

分 类 号：R286.0[医药卫生—中药学]