Citation: CHI Shuyao, WU Dike, SUN Jinhong, YE Ruhan, WANG Xiaoyan. Simultaneous determination of seven residual solvents in bovis calculus artifactus by headspace gas chromatography[J]. Chinese Journal of Chromatography, ;2014, 32(5): 553-557. doi: 10.3724/SP.J.1123.2014.01013 shu

Simultaneous determination of seven residual solvents in bovis calculus artifactus by headspace gas chromatography

CHI Shuyao ^1,2,, ,
WU Dike ¹ ,
SUN Jinhong ¹ ,
YE Ruhan ¹ ,
WANG Xiaoyan ¹

1.
1. Guangzhou PharmaLab Co. Ltd., Guangzhou 510070, China;

Corresponding author: CHI Shuyao,
Received Date: 7 January 2014
Available Online: 27 January 2014
Fund Project: 广东省科技计划项目(2012B040307002). (2012B040307002)

A headspace gas chromatography (HS-GC) method was developed for the simultaneous 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 separation and detection of the residual solvents, and the internal standard method was used for the quantification. The chromatographic conditions, such as equilibrium temperature and equilibrium time, were optimized. Under the optimized conditions, all of the seven residual solvents showed good linear relationships with good correlation coefficients (not less than 0.9993) 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 quantification (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.
- internal standard method,
- headspace gas chromatography (HS-GC),
- residual solvent,
- bovis calculus artifactus
1. [1]
  [1] Yang H W, Wang Z, Xin M T, et al. Chinese Traditional Patent Medicine (杨洪武, 王峥, 辛敏通, 等. 中成药), 2003, 25(4): 290
2. [2]
  [2] Luo X R, Cao H, Xing J B, et al. Pharmaceutical Journal of Chinese People’s Liberation Army (罗晓茹, 曹红, 邢俊波, 等. 解放军药学学报), 2009, 25(3): 247
3. [3]
  [3] Chinese Pharmacopoeia Commission. Chinese Pharmacopoeia: Part Ⅱ. Beijing: China Medical Science Press (国家药典委员会. 中华人民共和国药典: 2部. 北京: 中国医药科技出版社), 2010: Appendix 61
4. [4]
  [4] B’Hymer C. Pharm Res, 2003, 20(3): 337
5. [5]
  [5] Impurities: Guideline for Residual Solvents. International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use. 2009
6. [6]
  [6] Peng M, Liu J, Lu D, et al. J Chromatogr Sci, 2012, 50: 727
7. [7]
  [7] Saraji M, Khayamian T, Siahpoosh Z H, et al. Anal Methods, 2012, 4: 1552
8. [8]
  [8] Fang Q X, Diao X L, Wan Q H, et al. Journal of Instrumental Analysis (方秋雪, 刁兴利, 万谦宏, 等. 分析测试学报), 2013, 32(3): 308
9. [9]
  [9] Hu H L. Chinese Journal of Chromatography (胡慧廉. 色谱), 2012, 30(1): 99
10. [10]
  [10] Xu Y H, Zhu B H, Zhong X H, et al. Chinese Journal of Chromatography (许瑛华, 朱炳辉, 钟秀华, 等. 色谱), 2010, 28(1): 73
11. [11]
  [11] Lü Q, Zhang Q, Kang S Y, et al. Journal of Instrumental Analysis (吕庆, 张庆, 康苏媛, 等. 分析测试学报), 2011, 30(2): 171
12. [12]
  [12] Liu Y M, Ge N, Wang F, et al. Chinese Journal of Chromatography (刘永明, 葛娜, 王飞, 等. 色谱), 2012, 30(8): 782
13. [13]
  [13] Li P, Chi Y H, Chen D Y. Chinese Journal of Pharmaceutical Analysis (李平, 迟颖红, 陈东英. 药物分析杂志), 2008, 28(3): 427
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