HPLC同时测定小儿氨酚黄那敏制剂中的4种甜味剂

Simultaneous determination of four sweeteners in Pediatric paracetamol,atificial cow-bezoar and chlorphenamine maleate preparations by HPLC

目的采用HPLC法同时测定制剂中4种甜味剂(安赛蜜、糖精钠、阿司帕坦、甜菊苷)的含量。方法采用Agilent Zorbax SB-C_(18)色谱柱(250 mm×4.6 mm,5μm),流动相A为0.02 mol·L^(-1)磷酸二氢铵溶液(pH4.4),B为乙腈,梯度洗脱,流速1.0 mL·min^(-1),检测波长200 nm(糖精钠、阿司帕坦、甜菊苷)、226 nm(安赛蜜),柱温30℃,进样量10μL。结果安赛蜜、糖精钠、阿司帕坦、甜菊苷均达到基线分离,分离度符合要求,各辅料均无干扰,线性范围分别为1.012~404.800μg·mL^(-1)(r=0.9999)、1.117~223.400μg·mL^(-1)(r=0.9999)、1.180~471.800μg·mL^(-1)(r=0.9997)、0.605~605.200μg·mL^(-1)(r=0.9999);检测限分别为19.7、8.0、11.2、25.4 ng·mL^(-1);定量限分别为65.7、26.0、37.5、84.7 ng·mL^(-1);平均加样回收率分别为97.81%、98.30%、98.00%、101.10%,RSD分别为1.84%、1.39%、0.71%、1.98%(n=9)。结论所用方法稳定性、重复性均较好,通过测定甜味剂含量可监控制剂生产过程中辅料投料是否与处方一致,为儿童用药中甜味剂的质量控制提供了参考。

OBJECTIVE To determine sweeteners including potassium acesulfame,sodium saccharine,aspartame and stevioside in Pediatric paracetamol,atificial cow-bezoar and chlorphenamine maleate preparations by HPLC.METHODS The separation was conducted on an Agilent SB-Cis(250 mm×4.6 mm,5μm)column coupled with the detection wavelength setting at 200 nm for sodium saccharine,aspartame and stevioside,226 nm for potassium acesulfame.The mobile phase consisted of 0.02 mol·L^(-1)ammonium dihydrogensolution(pH4.4)(A)and acetonitrile(B)with gradient elution with The flow rate of 1.0 mL·min^(-1).The column temperature was 30 C and the injection volume was 10μL.RESULTS Good separation of 4 sweeteners and other excipients were achieved.The linear ranges of potassium acesulfame,sodium saccharinem,aspartame and stevioside were 1.012-404.800μg·mL^(-1)(r=0.999),1.117-223.400μg·mL^(-1)(r=0.9999),1.180471.800μg·mL^(-1)(r=0.9997),and 0.605-605.200μg·mL^(-1)(r=0.9999),respectively.The quantitation limits of detection 19.7 ng·mL^(-1)8.0 ng·mL^(-1),11.2ng·mL^(-1),and 25.4ng·mL^(-1),respectively.The limits of detection were 65.7 ng·mL^(-1),26.0ng·mL^(-1)37.5 ng·mL^(-1),and 84.7μg·mL^(-1),respectively.The average recoveries were 97.81%,98.30%,98.00%and 101.10%,with the RSDs of 1.84%,1.39%,0.71%,and 1.98%(n=9),respectively.CONCLUSION The method shows high selectivity and sensitivity.The determination results can be applied for monitoring of the manufacturing process.