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气相色谱测定大蒜素原料药中基因毒性杂质3-氯丙烯

Determination of genotoxic impurity 3 chloropropene in allicin API by gas chromatography
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摘要 目的:建立一种气相色谱法检测大蒜素中3-氯丙烯含量的方法。方法:采用Aglient DB WAX毛细管柱分离,FID检测器检测,3-氯丙烯的含量采用外标法计算。结果:3-氯丙烯质量浓度在0.003~0.060μL·mL^(-1)范围内与峰面积呈正相关(R^(2)=0.9998);检测限为0.0012μL·mL^(-1),定量限为0.003μL·mL^(-1);平均加样回收率为94.6217%;系统适应性、重复性、中间精密度、准确度、稳定性、耐用性试验的RSD值均小于5%。结论:建立气相色谱法为大蒜素原料药中是否残留起始物料3-氯丙烯提供了一种简单快速、灵敏度高、准确可靠方法。 Objective:Establish a method to detect the content of 3-chloropropylene in allicin by gas chromatography.Method:Aglient DB-WAX capillary column was used for separation,FID detector was used for detection,and the content of 3-allyl chloride was calculated using the external standard method.Result:The mass concentration of 3-chloropropene was positively correlated with the peak area within the range of 0.003~0.060μL·mL^(-1)(R^(2)=0.9998);the limit of detection was 0.0012μL·mL^(-1),and the limit of quantification was 0.003μL·mL^(-1);the average recoveries of the spiked samples were 94.6217%;and the RSD values of the system adaptability,repeatability,intermediate precision,accuracy,stability and durability tests were all less than 5%.Conclusion:The establishment of gas chromatography provides a simple,fast,highly sensitive,accurate and reliable method for whether the starting material 3-chloropropylene remains in allicin API.
作者 冯紫平 胡雅稳 甘若金 米雪 潘艳丽 张昊翔 张梦华 胡志林 Feng Zi-ping;Hu Ya-wen;Gan Ruo-jin;Mi Xue;Pan Yan-li;Zhang Hao-xiang;Zhang Meng-hua;Hu Zhi-lin(Xinjiang Huashidan Pharmaceutical Limited Company,Urumqi 830011,China)
出处 《北方药学》 2025年第10期4-7,共4页 Journal of North Pharmacy
基金 新疆维吾尔自治区重大科技专项项目(2022A03016) 兵团科技计划项目(2025YD023) 兵团科技计划项目(2022DB031)。
关键词 3-氯丙烯 气相色谱法 大蒜素 基因毒性 3-chloropropene gas chromatography allicin genotoxicity
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