【摘要】 建立了在线固相萃取-高效液相色谱法测定人体尿液中的N-乙酰-S-(N-甲基甲氨酰)半胱氨酸(AMCC)的分析方法。左泵以Amino Pac PA柱作为在线固相萃取柱、5 mmol/L KH2PO4溶液为流动相,将AMCC与样品基质分离;然后通过控制阀切换时间仅将含AMCC的部分样品溶液在线洗脱至Acclaim PAⅡC18分析柱上,右泵以0.1%H3PO4溶液(含5%乙腈)和乙腈为流动相对AMCC进行梯度洗脱分离和分析测定。结果表明,AMCC在1.0~100 mg/L范围内线性关系良好,相关系数r>0.999;上样量为10μL时,方法定量限为0.2 mg/L;回收率在85.9%~82.9%之间;相对标准偏差(n=6)分别为0.2%(保留时间)和4.0%(峰面积)。与传统的离线固相萃取-高效液相色谱法相比,本方法更为简便环保、高效稳定。用本方法测定了7份人体尿液,结果满意。更多还原

【Abstract】 A method was developed for the determination of N-acetyl-S-( N-methylcarbamoyl) cysteine( AMCC) in human urine by online solid-phase extraction( SPE)-high performance liquid chromatography( HPLC). The separation of AMCC from the urine matrix was performed on Amoni Pac PA Solid phase Extraction( SPE) column with 5 mmol / L KH2PO4 as the mobile phase by left pump. Then the time was controlled to switch the valve to make only the section of sample containing AMCC transferred into the analytic column-Acclaim PAⅡ C18. The determination was performed using gradient elution of 0.1% H3PO4( containing5% acetonitrile) and acetonitrile by right pump. The results showed that AMCC present good linear correlation in the range of 1. 0- 100 mg / L with a correlation coefficient of above 0. 999,the quantitation limit of the method was 0.2 mg / L( with the sample inject volume = 10 μL),the recoveries of spiked samples were in the range of 82.9%-85.9%,and the relative standard deviation( n = 6) of retention time and peak area were 0.2% and 4. 0% respectively. Compared with offline SPE-HPLC, the proposed method was convenient,environmentally friendly,efficient and stable,and feasible for the detection of AMCC in 7 human urine samples.更多还原