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作 者:何传昌[1] 关瑾[1] 丁爽[1] 阎峰[1] 石爽[1] 牛秋玲[1]
机构地区:[1]沈阳化工大学应用化学学院,辽宁沈阳110142
出 处:《沈阳药科大学学报》2013年第9期696-700,共5页Journal of Shenyang Pharmaceutical University
基 金:辽宁省教育厅科学研究一般项目(L2012150)
摘 要:目的建立分离分析5-氨基乙酰丙酸及4种相关组分的反相离子对液相色谱法。方法考察了缓冲溶液的pH值、离子对的种类和浓度等色谱条件对分离分析的影响。以乙腈-20mm01.L-1磷酸二氢钾(pH值2.0,含2.0mmol·L-1辛烷磺酸钠)为流动相,在ZORBAXSB—C18色谱柱上,采用梯度洗脱,对5-氨基乙酰丙酸及4种相关组分进行分离分析。结果在优化色谱条件下,5-氨基乙酰丙酸及4种相关组分在15min内达到基线分离;5-氨基乙酰丙酸质量浓度在0.1.2.0g·L-1内与峰面积呈良好的线性关系,相关系数为0.9995;检出限(信噪比为3)为3.0mg·L-1;样品的回收率为99.3%-100.5%,相对标准偏差为0.16%-0.92%。结论该方法操作简单、快速、准确可靠,可用于实际样品的分析,并获得了令人满意的结果。Objective To develop a method for the separation and determination of 5-aminolevulinic acid (ALA) and related four substances by reversed-phase ion-pair high performance liquid chromatography(RPIP-HPLC). Methods The influences of pH of buffer, type and concentration of ion-pair were investiga- ted by RPIP-HPLC on a ZORBAX SB- C18 column. The separation of the ALA and related four substances were studied using acetonitrile- 20 mmol. L -1 potassium dihydrogen phosphate ( containing 2. 0 retool. L - octanesulfonic acid sodium,pH 2. 0) as mobile phase with a gradient elution program and detection wave- length of 205 nm. Results Under the optimized condition, ALA and related four substances were baseline separated within 15 min. The calibration curve of ALA was good linear between the peak areas and the con- centrations of 0. 1- 2. 0 g. L - 1 with correlation coefficients r2 = 0. 999 5. The limit of detection ( SIN = 3 ) for ALA was 3.0 mg.L-1. The percentage recoveries were ranged from 99. 3% to 100. 5% with acceptable relative standard deviations of 0. 16 %- 0. 92 %. Conclusions The method is simple, sensitive, accurate and reliable for the determination of real samples.
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