反相离子对色谱法测定保健食品中硫酸软骨素和盐酸氨基葡萄糖

建立检测保健食品中硫酸软骨素和盐酸氨基葡萄糖含量的反相离子对色谱分析方法。称取样品,以乙腈/水(5/95,v/v)混合溶液进行超声提取,稀释定容后,滤过。采用高效液相色谱法进行测定,以Agilent Zorbax SB-Aq(4.6×250mm,5μm)色谱柱作为分析柱,柱温30℃,流速0.8mL/min,流动相为乙腈/10mmol/L戊烷磺酸钠溶液(5/95,v/v),等度洗脱,以外标法定量。硫酸软骨素和盐酸氨基葡萄糖分别在0.1~0.75mg/mL和0.2~1.5mg/mL的浓度范围内呈良好线性关系,相关系数R^(2)分别为0.995和0.998;硫酸软骨素加标回收率在101.2%~105.4%之间,精密度RSD为0.3%;盐酸氨基葡萄糖加标回收率在102.1%~106.0%之间,精密度RSD为0.3%。此方法操作简单,准确性好,重复性好,适用于保健食品中硫酸软骨素和盐酸氨基葡萄糖的含量测定。

Optimizing the Quadruple-potential Waveform for the Determination of Gentamicin Sulfate by High Performance Liquid Chromatography with Pulsed Electrochemical Detection

In this paper, a quadruple-potential waveform was investigated and optimized for the determination of gentamicin by reversed phase ion-pair chromatography. Instead of a relatively high positive potential, a negative potential was adopted as a potential for the cleaning of gold working electrode. By this way, the formation of gold oxide resulting from the application of high positive potential during the analyte detection and electrode cleaning was greatly reduced, and therefore, the dissolution and recession of gold working electrode was also reduced. The good condition of gold working electrode achieved by this quadruple-potential waveform can help us to obtain a good reproducibility. In order to acquire signal-to-noise ratio as high as possible, several waveform parameters affecting the detection of gentamicin were carefully selected. The analytical method has been applied to the determination of two real gentamicin samples, and good results with low relative standard deviation not more than 4% were obtained.

复方消毒液中双癸基二甲基氯化铵的高效液相色谱测定法

目的研究复方消毒液中双癸基二甲基氯化铵的高效液相色谱测定法。方法采用反相高效液相离子对色谱法,用带有蒸发光散射检测器的高效液相色谱仪对复方消毒液中双癸基二甲基氯化铵进行色谱分离和方法测定。结果流动相采用乙腈-0.1%三氟乙酸溶液(体积比为80∶20),检测器选择气体压力20 Psi、喷雾器级别50%、漂移管温度80℃等条件。在50～500 mg/L的线性范围内,r=0.999 2,方法的相对标准偏差为1.28%～2.19%,回收率为92%～101.4%,检测限为5.2μg/L。结论该方法色谱分离较好,分析速度较快,前处理简单,适用复方消毒液中双癸基二甲基氯化铵的测定。