藿香正气水中乙醇含量测定方法研究

2009年6月第1卷第6期中同现代中药 Modem Chinese MedicineJun, 2009 Vol 11 No藿香正气水中乙醇含量测定方法研究申放,黄婉峰,高卫东(佛山市药品检验所,广东佛山528000[摘要]目的:对霖香正气水中乙醇的含量测定方法进行改进。方法:色谱柱为 phenomenex毛细管柱nZB- waxplus(30mx0.25mm,0.25μm);氮气为载气,流速为0.5 mL min,分流比为30:1;进样口温度为90℃;柱温为85℃;FID检测器,温度为200℃;进样量0.1μL;正丙醇为内标物。结果:在该色谱条件下,歡香正气水中乙醇和内标物得到良好的分离,乙醇在0.010~0.1mL·mL线性良好(r=0.995,n=7);平均回收率为100.0%,RSD=1.18%(n=6)。结论:该法灵敏、准确,重复性好,可用于测定该制剂的乙醇含量关键香正气水;乙醇;气相色谱香正气水具有解表化湿,理气和中的功能,临床常用于外感风寒、内伤湿滞或夏伤暑湿所致的感冒等。对于制剂中乙醇含量的检查,《中国药典》中规定是以二乙烯苯乙基乙烯苯型高分子多孔小球作为载体的填充柱进行测定,但是因为填充柱有不适宜做程序升温以及相对理论塔板数比较低等不足,在药品检测工作中使用有减少的趋势,而多用毛细管柱。气相色谱毛细管柱因其高分离能力1.乙醉峰:2.丙酚峰高灵敏度、高分析速度等独特优点而得到迅速发展。A内标物正内醇:B.对照品:C香正气水供试品查阅文献未见有关于以聚乙二醇极性柱为色谱柱,图1气相色谱图采用氢火焰离子化检测器气相色谱法测定制剂中乙醇含量的报道,故本实验建立了相应方法,为乙醇2校正因子测定含量的测定提供参考。精密量取恒温至20℃的无水乙醇4,5,6mL,1仪器与试药分别置100m量瓶中,分别精密加入恒温至20℃的正内醇(内标物)5mL,加水稀释至刻度,取上述3Varian CP-3800气相色谱仪,FD检测器;phe种溶液适量,按上述色谱条件分别连续进样3次nonene聚乙二醇毛细管柱 zebron ZB-waxplus(30mx计算乙醇的校正因子为1.3904,RSD=1%6%。0.25mm,0.25μm)。无水乙醇,正丙醇均为分析2.3供试品溶液的制备纯,水为超纯水。藿香正气水,四川蜀中制约有限23供试品溶液的制备精密吸取恒温至20℃的本品溶液10mL,置公司(批号080302,080807,080923)。100mL量瓶中,精密加入恒温至20℃的正丙醇5mL2方法和结果加水稀释至刻度,摇匀,即得。2.1色谱条件与系统适应性试验2.4线性关系氢气流速为30 mL. min-',尾吹流速28mL·min精密量取恒温至20℃的无水乙醇1,2,氮气流速05mL·min1,空气流速为300mLm8,10mL,分别置100mL量瓶中,分别精密加入柱温为85℃;进样口温度为90℃,检测器温度为恒温至20℃的正丙醇(内标物)5mL,加水稀释至刻200℃,分流比为30:1。在此色谱条件下,乙醇和正度,摇匀,按上述色谱条件进样,每次进样0.lμ,丙醇有较好的分离,色谱图见图1。以对照品含量为橫坐标,以对照品峰面积与内标峰[通讯作者]‘高卫东,E-mail:weidong@163.com009年6月第卷第6期中国现代中药 Moclern Chinese medicineJun 2009 Vol 11 No 6面积之比为纵坐标,绘制标准曲线并得到回归方程,表1加样回收率试验Y=14.352X-0.0472,r=0.9995。样品含测得收率平均收RSD2.5精密度试验99.5700.0L.18精密量取恒温至20℃的无水乙醇5mL置100mL9.66100.87量瓶中,加入恒温至20咒℃的正丙醇5mL,用水稀释4.629624.629.5598.48刻度,摇匀。每次进样0.IμL,连续进样6次,计算校正因子,结果RSD=1.06%4.629.70101.73水乙醇加入量均为500mL2.6稳定性试验取同一批号的供试品溶液,照2.3制备供试品表2样品中乙醇含量测定溶液,精密吸取0.1μL,于0,1,2,3,5,6,12h乙醇平均含址08030245.5进样,测定,计算乙醇的含量,RSD=1.24%。结080807果表明,供试品溶液在12h内基本稳定。27重复性试验精密量取同一批号的恒温至20℃的样品6份,每讨论份10mL,加入恒温至20℃的正丙醇5mL,用水稀释至刻度,摇匀。按上述色谱条件测定,计算每份乙醇乙醇为极性物质,故选用极性柱。由于对照品溶液和样品溶液的含水量较大,因此用较小的进样的含量,平均为4.2%,RSD=015%,重复性较好。量,以免将FD灭火和对色谱柱产生损坏。因未见2.8回收率试验有文献报道采用FID检测器,以聚乙二醇极性毛细精密量取恒温至20℃的已知含量的相同样品6管色谱柱测定藿香正气水中乙醇的含量,故本文报份,每份10mL,置100mL量瓶中,精密加入恒温至道之。方法学考察证实此方法可行。内标法加校正20℃的无水乙醇5mL,再加入恒温至20的正内醇因子测定样品中乙醇的含量,操作较简便,分离效5mL,用水稀释至10mL,摇匀。按上述色谱条件测果好,分析时间短,结果准确可靠。cM定,记录色谱图,计算回收率,结果见表I。2.9样品测定参考文献精密吸取恒温至20℃的样品l0mL,加入恒温至[]国家药典委员会,中国药典(一部)[S].北京:化学工业20℃的正丙醇5mL,用水稀释至刻度,摇匀。按上出版社,2005:662述色谱条件测定并计算,结果见表2。(收稿日期2008-1203Improved Method for Determining Ethanol in Huo Xiang ZhengQiShuiFang, Huang Wanfeng, GaFoshan Institute for Drug control, Foshan Guangdong 528000, China)[Abstract]Objective: To improve the method for determining ethanol in Huo Xiang Zheng QiShui by GC.Methods: Chromatographic column was Phenomenex Zebron ZB-Waxplus(30m x0. 25mm, 0. 25 um), the carrier gaswas nitrogen, Alow rate was 0 5mL.min", split ratio was 30: 1. The column temperature was at 85C, inlet tempera-ture was 90C, FID detection was 200C, injection volume was 0. IuL The n-propanol was used as intemal substance. Results: The linearity of ethanol were good in the range of 0. 01-0. 1 mL.- with r=0. 999 5. The aver-age recovery of ethanol was 100. 0%, RSD was 1. 18%. Conclusion: This method is sensitive, rapid, accurate andreproducible, and can be used for the test of ethanol in Huo Xiang ZhengQiShui.I Key words] Huo Xiang ZhengQiShui; Ethanol; GC(E4%24 A)in characteristic fingerprints, and Similarity Evaluation system was applied to evaluate fingerprint of theten batches of Herba Andrographis, the total content of andrographolide and dehydroandrographolide was between1. 09% and 4. 47%. Conclusion: The method is sensitive, repeatable and accurate, which can be used as qualitycontrol for Herba Andrographis and has been used in Hong Kong Chinese Materia Medica Standards. We suggest thatthe HPLC fingerprinting should be involved in the quality control of Herba Andrographis, and the total content of andrographolide and dehydroandrographolide in Herba Andrographis is not less than 1. 0%Key words] Quality assessment; Herba Andrographis; HPLC fingerprint; Content determination