气相色谱法同时测定麝香追风止痛膏中5种挥发性成分的含量 点击下载
论文标题: 气相色谱法同时测定麝香追风止痛膏中5种挥发性成分的含量
英文标题:
中文摘要: 目的:建立同时测定麝香追风止痛膏中5种挥发性成分含量的方法。方法:采用气相色谱法,色谱柱为PEG-20M毛细管柱,检测器为氢火焰离子化检测器,载气为氮气(纯度:99.999%),柱流量为1.5 mL/min,吹扫流量为3.0 mL/min,分流比为5 ∶ 1,进样口温度为200 ℃,检测器温度为250 ℃,程序升温,进样量为2 μL,尾吹流量为40 mL/min。结果:樟脑、龙脑、异龙脑、薄荷脑、水杨酸甲酯检测质量浓度线性范围分别为19.78~247.26 μg/mL(r=0.999 6)、15.88~198.52 μg/mL(r=0.999 9)、8.60~107.56 μg/mL(r=0.999 9)、20.11~251.32 μg/mL(r=0.999 8)、12.09~151.11 μg/mL(r=0.999 3);定量限分别为329.68、264.69、143.41、335.09、402.96 ng/mL,检测限分别为98.90、79.41、43.02、100.53、120.89 ng/mL;中间精密度、稳定性、重复性试验的RSD均小于3%;加样回收率分别为97.85%~101.52%(RSD=1.54%,n=6)、99.55%~103.75%(RSD=1.38%,n=6)、98.88%~104.23%(RSD=1.94%,n=6)、 98.11%~102.64%(RSD=1.92%,n=6)、96.55%~99.61%(RSD=1.44%,n=6);耐用性试验的RSD均小于3%。结论:该方法操作简便,精密度、稳定性、重复性、耐用性好,可用于麝香追风止痛膏中5种挥发性成分含量的同时测定。
英文摘要: OBJECTIVE: To establish the method for simultaneous determination of 5 volatile constituents in Shexiang zhuifeng zhitong plaster. METHODS: Gas chromatography was adopted. The determination was performed on PEG-20M capillary column with flame ionization detector as detector,nitrogen (99.999%) as carrier gas, with column flow rate of 1.5 mL/min, purge flow of 3.0 mL/min, split ratio of 5 ∶ 1, injector temperature of 200 ℃, detector temperature of 250 ℃, temperature programming, sample size of 2 μL, tail blowing flow of 40 mL/min. RESULTS: The linear range of camphor, borneol, isoborneol, menthol and  menthyl salicylate were 19.78-247.26 μg/mL(r=0.999 6), 15.88-198.52 μg/mL (r=0.999 9), 8.60-107.56 μg/mL(r=0.999 9), 20.11-251.32 μg/mL (r=0.999 8)and 12.09-151.11 μg/mL (r=0.999 3), respectively. The limits of quantitation were 329.68,264.69, 143.41, 335.09, 402.96 ng/mL; the limits of detection were 98.90, 79.41, 43.02, 100.53, 120.89 ng/mL, respectively. RSDs of precision, stability and reproducibility tests were all lower than 3%. The recoveries were 97.85%-101.52%(RSD=1.54%,n=6),  99.55%-103.75%(RSD=1.38%,n=6), 98.88%-104.23%(RSD=1.94%,n=6), 98.11%-102.64%(RSD=1.92%,n=6), 96.55%-99.61%(RSD=1.44%,n=6), respectively. RSDs of durability test were all lower than 3%. CONCLUSIONS: The method is simple, precise, stable,reproducible and durable, and can be used for simultaneous determination of 5 volatile constituents in Shexiang zhuifeng zhitong plaster.
期刊: 2018年第29卷第14期
作者: 黄传俊,陈云,曾博程,刘勇,曾凡华,王文娟,叶修文,杜君,代晓进,杨红菊,谯志文,周年华
英文作者: HUANG Chuanjun,CHEN Yun,ZENG Bocheng,LIU Yong,ZENG Fanhua,WANG Wenjuan,YE Xiuwen,DU Jun,DAI Xiaojin,YANG Hongju,QIAO Zhiwen,ZHOU Nianhua
关键字: 麝香追风止痛膏;樟脑;龙脑;异龙脑;薄荷脑;水杨酸甲酯;气相色谱法;含量测定
KEYWORDS: Shexiang zhuifeng zhitong plaster; Camphor; Borneol; Isoborneol; Menthol; Menthyl salicylate; GC; Content determination
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