蒸发光散射检测器的清洗方法

目的建立一种蒸发光散射检测器的清洗方法。方法在高温氮气流的作用下,利用高浓度的盐酸溶液去除蒸发光散射检测器蒸发管内壁的奶垢;依次用丙酮、乙腈、甲醇、水溶液清洗之后,高温氮气流的作用下继续烘烤;清洗结束后,对蒸发光散射检测器进行面积归一化。结果乳糖在0～4mg/mL范围内,浓度与峰面积采用幂函数方程绘制标准曲线,相关系数大于0.99,检出限为190 mg/100 g;样品的加标平均回收率为96.45%～103.16%,相对标准偏差为3.88%～5.18%;对清洗前后的蒸发光散射检测器进行10次重复性测试,相对标准偏差为0.66%,清洗后检测信号增大2倍,仪器噪音减少4倍。结论本方法适用于蒸发光散射检测器的彻底清洗,可以减少更换蒸发管的次数。

Cleaning method of evaporative light scattering detector

Objective To establish a cleaning method for evaporative light scattering detector. Method The high-concentration hydrochloric acid solution was used to remove the scale of the inner wall of the evaporation tube of the evaporative light scattering detector under the action of a high-temperature nitrogen stream. After washing with acetone, acetonitrile, methanol, and aqueous solution in sequence, the evaporation tube of the evaporative light scattering detector was continued to be baked under the action of high-temperature nitrogen gas. After the cleaning was completed, the area of the evaporative light scattering detector was normalized. Result When lactose was in the range of 0?4 mg/m L, the concentration curve and the peak area were plotted by the power function equation. The correlation coefficient was greater than 0.99, and the limit of detection was 190 mg/100 g. The average recoveries of the sample were 96.45%?103.16%, and the relative standard deviations were 3.88%?5.18%. The evaporative light scattering detector before and after cleaning was carried out for 10 times, the relative standard deviation was 0.66%, the detection signal was increased by 2 times after cleaning, and the instrument noise was reduced by 4 times. Conclusion The method is suitable for thorough cleaning of the evaporative light scattering detector and able to reduce the replacement time of the evaporation tube.