建立了同时测定人工牛黄中石油醚（60~90℃）、丙酮、乙酸乙酯、甲醇、二氯甲烷、乙醇、乙酸丁酯7种残留溶剂的顶空气相色谱分析方法。以 Agilent DB-WAX 毛细管色谱柱为分离柱，氢火焰离子化检测器检测，内标法定量，并考察了顶空平衡温度、加压时间、平衡时间等对残留溶剂测定的影响。在优化的条件下，7种残留溶剂在选择的浓度范围内线性关系良好，相关系数（ r）均不小于0.9993；在高、中、低3个加标水平下，平均回收率为94.7％~105.2％，相对标准偏差（RSD）均不大于3.5％。方法的检出限（LOD）为0.43~5.23 mg/L，定量限（LOQ）为1.25~16.67 mg/L。该方法操作简单、准确灵敏、高效快捷，适用于人工牛黄中7种残留溶剂的同时检测。
A headspace gas chromatography( HS-GC)method was developed for the simulta-neous determination of seven residual solvents( petroleum ether( 60-90 ℃),acetone,ethyl acetate,methanol,methylene chloride,ethanol and butyl acetate)in bovis calculus artifactus. The DB-WAX capillary column and flame ionization detector( FID)were used for the separa-tion and detection of the residual solvents,and the internal standard method was used for the quantification. The chromatographic conditions,such as equilibrium temperature and equilibri-um time,were optimized. Under the optimized conditions,all of the seven residual solvents showed good linear relationships with good correlation coefficients( not less than 0. 999 3)in the prescribed concentration range. At three spiked levels,the recoveries for the seven residual solvents were 94. 7%-105. 2% with the relative standard deviations( RSDs)less than 3. 5%. The limits of detection( LODs)of the method were 0. 43-5. 23 mg/L,and the limits of quantifica-tion( LOQs)were 1. 25-16. 67 mg/L. The method is simple,rapid,sensitive and accurate,and is suitable for the simultaneous determination of the seven residual solvents in bovis calculus artifactus.
参考文献
| [1] | 杨洪武;王峥;辛敏通.[J].中成药,200325(04):290. |
| [2] | 罗晓茹;曹红;邢俊波.[J].解放军药学学报,200925(03):247. |
| [3] | 国家药典委员会.中华人民共和国药典:2 部[M].北京:中国医药科技出版社,2010:Appendix61. |
| [4] | B'Hymer C.[J].Pharmaceutical Research,200320(03):337. |
| [5] | ImpuritiesGuideline for Residual Solvents.[A].,2009 |
| [6] | Peng M;Liu J;Lu D.[J].Journal of Chromatography Science,201250:727. |
| [7] | Saraji M;Khayamian T;Siahpoosh Z H.[J].Anal Meth-ods,20124:1552. |
| [8] | 方秋雪;刁兴利;万谦宏.[J].分析测试学报,201332(03):308. |
| [9] | 胡慧廉.[J].色谱,201230(01):99. |
| [10] | 许瑛华;朱炳辉;钟秀华.[J].色谱,201028(01):73. |
| [11] | 吕庆;张庆;康苏媛.[J].分析测试学报,201130(02):171. |
| [12] | 刘永明;葛娜;王飞.[J].色谱,201230(08):782. |
| [13] | 李平;迟颖红;陈东英.[J].药物分析杂志,200828(03):427. |
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