摘要
目的 建立顶空-气相色谱法测定小儿化痰止咳糖浆中乙醇及三氯甲烷含量.方法 采用DB-624毛细管色谱柱(SN:USR593111J),载气为氮气,顶空进样,进样口温度:200℃,程序升温:初始温度为60℃,保持8 min,以每分钟8℃的速率升温至120℃维持15 min,顶空瓶平衡温度为80 ℃,平衡时间为30 min;分流进样,分流比为10∶1,氢火焰离子化检测器(FID),检测器温度为250℃.结果 乙醇和三氯甲烷进样量分别在0.103～4.120 mg(r=0.999)和0.010～0.400 mg(r=0.999)范围内与峰面积呈良好的线性关系;精密度RSD分别为1.02％、1.26％;重复性的RSD分别为1.86％、1.97％;定量限分别为1.72 μg和30.86 μg,平均回收率分别为102％和99％,RSD分别为1.83％(n=6)和3.52％(n=6);来自2个厂家共6批样品,乙醇和三氯甲烷均超出现行药典规定限度.结论 本研究建立的方法专属性强,灵敏度高,适用性好,可以用于测定小儿化痰止咳糖浆中乙醇和三氯甲烷的含量.
Abstract
OBJECTIVE To establish a headspace GC method for determination of ethanol and chloroform in XiaoEr HuaTan ZhiKe Syrup.METHODS A DB-624(SN:USR593111J)column was used with nitrogen as the carrier gas.Headspace injection was applied with the injection port temperature at 200 ℃.The column temperature program was set as:remaining the starting temperature of 60 ℃ for 8 min,then increasing to 120 ℃ at the rate of 8℃/mnin and remaining 120℃ for 15 min.The detector temperature was 250 ℃,the headspace equilibrium tempera-ture was 80 ℃,and the equilibration time was 30 min,the injection split was 10∶1.An FID was uesd as the detector with the temperature at 250 ℃.RESULTS The linear range of ethanol fell into 0.103-5.131 mg(r=0.999)and chloroform fell into 0.57-28.65 μg(r=0.999);The RSD of precision were 1.02％and 1.26％;and the RSD of re-peatability were 1.86％and 1.97％;The limits of quantitation were 1.72 µg and 30.86 µg;The average recoveries were 102％and 99％(n=6,RSD were 1.83％and 4.52％).Six batches of ethanol and chloroform from two manu-facturers exceeded the limits.CONCLUSION The establisded method has the high sensitivity,good specificity and good applicability.It can be applicable to the determination of residuai ethanol and chloroform.
维普
万方数据