气相色谱法测定泊洛沙姆中抗氧剂二丁基羟基甲苯的含量

Determination of antioxidant butylated hydroxytoluene in poloxamer by gas chromatography

目的:采用气相色谱法测定药用辅料泊洛沙姆中抗氧剂二丁基羟基甲苯的含量。方法:采用VF-17ms色谱柱(30 m×0.53 mm×1.0μm,检测器温度:290℃,进样口温度:270℃),氢火焰离子化检测器,外标法定量测量二丁基羟基甲苯。结果:二丁基羟基甲苯线性范围为5~30μg·mL-1,r=0.9999;泊洛沙姆188中平均回收率为103.3%,RSD=1.24%;泊洛沙姆407中平均回收率为99.83%,RSD=3.28%。经测定,市售不同厂家及型号泊洛沙姆中均含有抗氧剂二丁基羟基甲苯,验证该检测的必要性,其含量范围为0.009%~0.014%。结论:本试验建立的气相测定方法可用于泊洛沙姆中抗氧剂二丁基羟基甲苯的检测,并为其质量管理和控制提供参考。

Objective:To establish a GC method for determination of butylated hydroxytoluene in pharmaceutical excipients Poloxamer 188 and 407.Methods:The test was performed in VF-17ms capillary column(30 m×0.53 mm×1.0μm,detector temperature:290℃,injection temperature:270℃).The hydrogen flame ionization detector(FID)was used and the external standard method was adopted to calculate the content of butylated hydroxytoluene.Results:The linear range of butylated hydroxytoluene fell into 5-30μg·mL-1 with r=0.9999.The average recovery of butylated hydroxytoluene in Poloxamer 188 was 103.3%,with RSD of 1.24%,and the average recovery of butylated hydroxytoluene in Poloxamer 407 was 99.83%with RSD of 3.28%.The test results showed that the antioxidant of butylated hydroxytoluene existed in all the samples from the different manufacturers.The contents of butylated hydroxytoluene fell into 0.009%-0.014%.That confirmed the necessity of the test.Conclusion:The established GC method can be used for determination the antioxidant butylated hydroxytoluene in poloxamer.That provides the reference for its quality management and control.