高聚物型色谱柱分离乙酰半胱氨酸及其有关物质

考察高聚物型色谱柱(聚苯乙烯-二乙烯基苯(PS-DVB)麦科菲反相高效液相色谱柱,MKF-RP-MH)分离乙酰半胱氨酸以及有关物质的适用性。采用MKF-RP-MH色谱柱(4.6×250 mm,5μm),V(0.02 mol/L的磷酸盐缓冲液(pH 3.0))∶V(乙腈)=9∶1为流动相,流速为1 mL/min,检测波长210 nm,柱温为25℃。乙酰半胱氨酸峰与有关物质峰的分离度均大于1.5;乙酰半胱氨酸质量浓度在11~111 mg/L的范围内,具有良好的线性关系,回归方程为A=18.195ρ+0.5229,r=0.9995(n=8);乙酰半胱氨酸的定量限为11 mg/L;最低检测限为0.035μg;进样精密度RSD=0.24%(n=6)。

Detection of relevant substances from acetylcysteine by HPLC

To review the applicability of determination of relevant substances in acetylcysteine by HPLC with polystyrene-divinylbenzene (PS-DVB) resin (MKF-RP-MH). The MKF-RP-MH (250 mm×4.6 mm, 5 μm) column was used. The mobile phase was 0.02 mol/L phosphate buffer (pH 3.0): acetonitrile (9∶1, V/V), the flow rate was 1.0 mL/min, the detection wavelength was set at 210 nm, and column temperature was set at 25 ℃. The resolution between the acetylcysteine peak and relevant substances were not less than 1.5. The calibration curve was in good linearity within the range of 11～111 mg/L with the regression equation of A=185.94ρ+0.0548, r=0.9996 (n=8). The quantitation limit was 11 mg/L, and the detection limit was 0.035 μg. The precision of the method was 0.24% (n=6).