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小儿化痰止咳糖浆中乙醇和三氯甲烷含量研究

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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.
Determination of Residual Ethanol and Chloroform in XiaoEr HuaTan ZhiKe Syrup
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.

XiaoEr HuaTan ZhiKe SyrupEthanolChloroformHeadspace GCResidual solvent

孟庆山、马芳芳、刘雪

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威海市食品药品检验检测研究院,山东威海 264210

小儿化痰止咳糖浆 乙醇 三氯甲烷 顶空气相色谱法 残留溶剂

2024

海峡药学
中国药学会福建分会

海峡药学

影响因子:0.643
ISSN:1006-3765
年,卷(期):2024.36(10)