葛根饮片的脱硫工艺研究

Study on Sulfur Dioxide Removal in Radix Puerariae by Ultrasonic Treatment

建立葛根饮片中二氧化硫残留量的含量测定方法,以5%Na HCO3溶液为脱硫液,考察用超声波处理脱除葛根饮片中二氧化硫的工艺。采用离子色谱法测定二氧化硫残留量,色谱柱为Dionex Ionpac AS11A阴离子色谱柱,流动相为10 mmol/L KOH溶液,体积流量为1. 0 m L/min,柱温30℃,进样量20μL。在单因素试验的基础上确定液料比、超声波功率和超声处理时间为考察因素,以二氧化硫残留量为考察指标,兼顾葛根素的损失率,采用正交实验设计优化脱硫工艺。葛根饮片中二氧化硫残留量的线性范围为1. 0~50. 0 mg/L(r=0. 999 8),重复性、精密度和稳定性试验的RSD均小于5%(n=6),加样回收率为95. 53%~102. 77%(RSD为1. 52%,n=9)。最优脱硫工艺为按液料比10∶1加入5%Na HCO3溶液,超声波功率135 W处理8 min,可去除70%以上的二氧化硫残留,过程中葛根素损失不超过10%。二氧化硫为水溶性物质,葛根素在水中微溶,文章兼顾葛根素的损失率和二氧化硫残留量的脱除率,优化脱硫工艺。建立的检测方法简单准确,适用于葛根中二氧化硫残留量的检测。脱硫方法简便可行,易于推广,为葛根饮片的安全使用提供参考,该研究也为药效成分具有类似理化性质的中药脱硫工艺设计提供思路。

To study the removal of sulfur dioxide in Radix Puerariae with 5%Na HCO3 by the method of ultrasonic treatment,the sulfur dioxide residue in Radix puerariae was separated on a Dionex Ionpac AS11 A ion exchange column using 10 mmol/L KOH as mobile phase with a flow rate of 1.0 m L/min.The sample size was 20μL and column temperature was 30°C.The liquid to material ratio,ultrasonic time and ultrasonic power were identified as influence factors on the basis of single factor experiments.Using the removal rate of sulfur dioxide residues and the loss rate of Puerarin in Radix puerariae as index,the extraction technique was optimized by orthogonal test.The linear range of sulfur dioxide residue was 1.0~50.0 mg/L(r=0.999 8)and the average recoveries were 95.53%~102.77%(RSD was 1.52%,n=9).RSDs of reproducibility,stability and precision tests were lower than 5%(n=6).The optimal extraction technique of removal of sulfur dioxide included adding 5%Na HCO3 with liquid to material ratio 10∶1(m L/g),ultrasonic for 8 min and ultrasonic power 135 W,and the final removal of sulfur dioxide yield was more than 70%and the loss rate of puerarin was less than 10%.Sulphur dioxide is soluble in water and Puerarin is slightly soluble in water,which makes the design of desulfurization process more difficult.The loss rate of Puerarin and the removal rate of sulfur dioxide residues in Radix puerariae were both considered to optimize desulfurization process.Removal of sulfur dioxide residues was as much as possible on the basis of the loss rate of Puerarin was as little as possible.The established determination method is simple,stable,accurate and suitable for the determination of sulfur dioxide in Radix puerariae.The optimal technique of sulfur dioxide removal is stable,and feasible.It provides ideas for desulfurization process design of active ingredient with similar physical and chemical properties in sulfur-fumigated traditional Chinese medicine.