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

所屬欄目:分析與測試

氣相色譜法測定和厚樸酚原料藥中殘留溶劑的研究
陳莉莉1,楊云霞2,門(mén) 靖3 (1. 陜西大河藥業(yè)有限責任公司,陜西 西安 710200;2. 陜西省藥品和疫苗檢查中心咸陽(yáng)分中心,陜西 咸陽(yáng) 712000;3. 西安萬(wàn)隆制藥股份有限公司,陜西 西安 710119)
摘 要:采用氣相色譜法,以二甲基亞砜為溶劑,頂空進(jìn)樣,以DB-624毛細管柱程序升溫,FID檢測器,建立了和厚樸酚中乙醇、二氯甲烷、正己烷等殘留溶劑的測定方法。結果表明:乙醇在2.500 4~750.120 μg/mL范圍線(xiàn)性方程為y=0.800 9x+4.133 2,相關(guān)系數0.999 1,線(xiàn)性良好;二氯甲烷在2.422~90.825 μg/mL范圍線(xiàn)性方程y=0.894 2x-0.639,相關(guān)系數0.999 5,線(xiàn)性良好;正己烷在0.096 469~43.845 μg/mL范圍線(xiàn)性方程為y=42.072x-29.422,相關(guān)系數0.995 5,線(xiàn)性良好。所建立的方法靈敏度高,準確性好,操作簡(jiǎn)便,適用于和厚樸酚殘留溶劑的測定。
關(guān)鍵詞:和厚樸酚;殘留溶劑;頂空進(jìn)樣;氣相色譜法
中圖分類(lèi)號:R284.1  文獻標識碼:A  文章編號: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
作者簡(jiǎn)介:陳莉莉(1980—),女,陜西蒲城人,主管藥師,執業(yè)藥師,研究方向:醫藥研發(fā)、植物提取及中藥化學(xué)研究(E-mail:695766755@qq.com)。
收稿日期:2022-04-19
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