顶空气相色谱法同时测定环维黄杨星D中四种有机溶剂残留量的研究
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摘要
目的建立测定环维黄杨星D中环己烷、丙酮、甲醇、三氯甲烷4种残留溶剂的检测方法。方法采用顶空气相色谱法测定。毛细管色谱柱为AgilentDB-WAX柱(30.0m×0.32mm×0.25μm),进样口温度为150℃;柱温程序为首先在40℃下保持5min,以10℃·min~(-1)的速率升温至100℃,再以35℃·min~(-1)的速率升温至200℃,保持1min;氢火焰离子化检测器(FID)温度为220℃;载气为高纯氮气,流速为32.5mL·min~(-1),分流比10∶1;顶空平衡温度为85℃,平衡时间为30min,传输管温度为110℃,进样环温度为105℃。结果在本色谱条件下,各残留溶剂均可基线分离。测得环己烷、丙酮、甲醇、三氯甲烷分别在168.947～275.789mg·L~(-1)、210.835～843.341mg·L~(-1)、206.157～824.627 mg·L~(-1)、1.988～7.952mg·L~(-1)范围内线性关系良好。环己烷、丙酮、甲醇和三氯甲烷的平均回收率分别为96.93%(n=6)、98.95%(n=6)、100.99%(n=6)、99.73%(n=6)。结论该气相色谱法操作简便、准确度、灵敏度高,可用于环维黄杨星D中残留溶剂的测定。
Objective To establish a method for determination of the four residual organic solvents, including cyclohexane,acetone, methanol, trichlormethane, in Cyclovirobuxinum D. Methods Gas headspace chromatography was applied to this study. The column was Agilent DB-WAX capillary column (30.0 m ×0.32 mm ×0.25μm) and the inlet temperature was 150℃. The Column gradient temperature was as folloes: 40℃ for 5 min, to 100℃ at the rate of 10℃·min~(-1), to 200℃ at the rate of 35℃·min~(-1) and then constant for 1 min. The temperature of flame ionization detector(FID) was set at 220℃. High purity nitrogen was used as the carrier gas, the flow rate was 32.5 mL·min~(-1), and the split ratio was 10∶1. The equilibrium temperature of headspace was 85℃, and the equilibrium time was 30 min. The temperature of transferring tube was 110 ℃, and the temperature of sampling ring was 105℃. Resu1 ts Under the conditions established in the present study,the baseling separation could be achieved for all tested residual solvents.Good linear relationships were established within the range of 168.947～275.7 8 9 mg·L~(-1),210.835～843.341 mg·L~(-1),206.157～824.627 mg·L~(-1) and 1.988～7.952 mg·L~(-1) for cyclohexane,scetone, ethanol and trichlormethane,respectively.The average recoveries of cyclohexane, acetone, ethanol and trichlormethane were 96.93 %(n=6), 98.95 %(n=6), 100.99 %(n=6) and 99.73 %( n = 6) respectively. Conc1 usion The method developed in the present study is simple and with sufficient accuracy and sensitivity for the determination of residual solvents in Cyclovirobuxinum D.
Objective To establish a method for determination of the four residual organic solvents, including cyclohexane,acetone, methanol, trichlormethane, in Cyclovirobuxinum D. Methods Gas headspace chromatography was applied to this study. The column was Agilent DB-WAX capillary column (30.0 m ×0.32 mm ×0.25μm) and the inlet temperature was 150℃. The Column gradient temperature was as folloes: 40℃ for 5 min, to 100℃ at the rate of 10℃·min~(-1), to 200℃ at the rate of 35℃·min~(-1) and then constant for 1 min. The temperature of flame ionization detector(FID) was set at 220℃. High purity nitrogen was used as the carrier gas, the flow rate was 32.5 mL·min~(-1), and the split ratio was 10∶1. The equilibrium temperature of headspace was 85℃, and the equilibrium time was 30 min. The temperature of transferring tube was 110 ℃, and the temperature of sampling ring was 105℃. Resu1 ts Under the conditions established in the present study,the baseling separation could be achieved for all tested residual solvents.Good linear relationships were established within the range of 168.947～275.7 8 9 mg·L~(-1),210.835～843.341 mg·L~(-1),206.157～824.627 mg·L~(-1) and 1.988～7.952 mg·L~(-1) for cyclohexane,scetone, ethanol and trichlormethane,respectively.The average recoveries of cyclohexane, acetone, ethanol and trichlormethane were 96.93 %(n=6), 98.95 %(n=6), 100.99 %(n=6) and 99.73 %( n = 6) respectively. Conc1 usion The method developed in the present study is simple and with sufficient accuracy and sensitivity for the determination of residual solvents in Cyclovirobuxinum D.
引文
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8伍乃英,郭青,吴晓燕.环维黄杨星D中有机溶剂残留量的测定[J].中国中医药咨询,2010,2(9):182
9王发,王嫦鹤,王莉,等.顶空毛细管气相色谱法测定奥硝唑原料的溶剂残留[J].西北药学杂志,2016,31(2):146
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11张贝,杨姗姗,王裴珮,等.顶空气相色谱法测定ET-26盐酸盐中的7种残留溶剂[J].华西药学杂志,2017,32(1):77
12中国药典2015年版.四部[S].2015:105
2梁秉文,邓晨安,王学斌,等.黄杨木生物碱Ⅰ、Ⅱ、Ⅲ、Ⅳ的分离与结构研究[J].中国药学杂志,1981,16(4):3
3胡国强,许启泰,张保国,等.环维黄杨星D分离方法改进[J].中国天然药物,2004,2(3):155~156
4马成芳,徐勇,张荣桂.黄杨宁提取工艺的改进[J].中国野生植物资源杂志,1996,(4):36
5袁明铭,王永金,夏介英,等.环维黄杨星D对大鼠原代心肌细胞缺氧复氧损伤的影响[J].现代中药研究与实践,2016,30(2):25
6黄丹丹,林玲,许立.环维黄杨星D对心衰大鼠心肌损伤及氧化应激的影响[J].中国药业,2014,23(19):26
7黄丹丹,邵靓婧,许立.环维黄杨星D对大鼠心力衰竭的治疗作用[J].医药导报,2014,12(33):1562
8伍乃英,郭青,吴晓燕.环维黄杨星D中有机溶剂残留量的测定[J].中国中医药咨询,2010,2(9):182
9王发,王嫦鹤,王莉,等.顶空毛细管气相色谱法测定奥硝唑原料的溶剂残留[J].西北药学杂志,2016,31(2):146
10姚静,吴建敏,高家敏,等.顶空GC测定缬沙坦原料有机溶剂残留量[J].中国药事,2009,23(7):681
11张贝,杨姗姗,王裴珮,等.顶空气相色谱法测定ET-26盐酸盐中的7种残留溶剂[J].华西药学杂志,2017,32(1):77
12中国药典2015年版.四部[S].2015:105