第 52 卷第 4 期Vol. 52 No. 4
2022 年 8 月Aug 2022

所属栏目:分析与测试

气相色谱法测定和厚朴酚原料药中残留溶剂的研究
陈莉莉1,杨云霞2,门 靖3 (1. 陕西大河药业有限责任公司,陕西 西安 710200;2. 陕西省药品和疫苗检查中心咸阳分中心,陕西 咸阳 712000;3. 西安万隆制药股份有限公司,陕西 西安 710119)
摘 要:采用气相色谱法,以二甲基亚砜为溶剂,顶空进样,以DB-624毛细管柱程序升温,FID检测器,建立了和厚朴酚中乙醇、二氯甲烷、正己烷等残留溶剂的测定方法。结果表明:乙醇在2.500 4~750.120 μg/mL范围线性方程为y=0.800 9x+4.133 2,相关系数0.999 1,线性良好;二氯甲烷在2.422~90.825 μg/mL范围线性方程y=0.894 2x-0.639,相关系数0.999 5,线性良好;正己烷在0.096 469~43.845 μg/mL范围线性方程为y=42.072x-29.422,相关系数0.995 5,线性良好。所建立的方法灵敏度高,准确性好,操作简便,适用于和厚朴酚残留溶剂的测定。
关键词:和厚朴酚;残留溶剂;顶空进样;气相色谱法
中图分类号:R284.1  文献标识码:A  文章编号:1009-9212(2022)04-0084-05
Determination of Residual Solvents in Honokiol by Gas Chromatography
CHEN Li-li1, YANG Yun-xia2, MEN Jing3 (1. Shaanxi Dahe Pharmaceutical Co., Ltd., Xi’an 710200, China; 2. Xianyang Branch of Shaanxi Province Drug and Vaccine Inspection Center, Xiangyang 712000, China; 3. Xianyang Wanlong Pharmaceutical Co., Ltd., Xi’an 710119, China)
Abstract:In a gas chromatography method, using the dimethyl sulfoxide as solvent, adopting the headspace sampling method, raising the temperature through DB-624 capillary column program, FID as the detector, the residual solvent such as ethanol, dichlormethane and n-hexane in honokiol was detected. The results showed that: the linear equation was expressed as y=0.800 9x+4.133 2 when ethanol is in the range of 2.500 4~750.120 μg/mL, the correlation coefficient reached 0.999 1, showing good linearity. The linear equation was expressed as y=0.894 2x-0.639 when dichloromethane falled in the range of 2.422~90.825 ug/mL, the correlation coefficient reached 0.999 5, with good linearity. And it was expressed as y=42.072x-29.422 when n-hexane falled in the range of 0.096 469~43.845 μg/mL, also showing the correlation coefficient of 0.995 5 and good linearity. This method was suitable for the determination of honokiol and honokiol residual solvents with the advantages including high sensitivity, good accuracy and simple operation.
Key words:honokiol; residual solvent; headspace sampling; gas chromatography method
作者简介:陈莉莉(1980—),女,陕西蒲城人,主管药师,执业药师,研究方向:医药研发、植物提取及中药化学研究(E-mail:695766755@qq.com)。
收稿日期:2022-04-19