Simultaneous determination of seven aconitum alkaloids in biological samples by liquid chromatography-linear ion trap multistage mass spectrometry coupled with on-line solid phase extraction

doi:10.3724/SP.J.1123.2015.10044

Abstract

Abstract:

An analytical method has been developed for the simultaneous determination of seven aconitum alkaloids in biological samples by liquid chromatography-linear ion trap multistage mass spectrometry (LC-LIT/MSⁿ) coupled with on-line solid phase extraction (on-line SPE). Mass fragmentation regularities of the seven aconitum alkaloids are discussed and summarized according to the analysis of their MSⁿ fragments. The samples were treated with acetonitrile for protein precipitation, followed by dilution and centrifugation. The resulting solution was injected into the LC system directly and processed by Waters Oasis^® HLB on-line SPE column for enrichment and purification. Chromatographic separation was performed on an Accucore C18 column using mobile phases of 0.01 mol/L ammonium acetate aqueous solution and methanol (both containing 0.1%(v/v) formic acid) for gradient elution. The analytes were detected in consecutive reaction monitoring (CRM) mode through positive electrospray ionization (ESI⁺). The calibration curves of the analytes within the investigated mass concentration ranges were fitted by second-order equations weighted 1/x, with r² ranging from 0.9991 to 0.9999. The method detection limits were 0.02-0.60 ng/mL for whole blood and urine, 0.02-0.40 ng/g for liver tissue. The recoveries at three spiked levels were within 91.1%-104.7%for all the analytes, with 0.2%-10.7%of intra-day RSDs and 1.0%-13.7%of inter-day RSDs (n=6). The established method is simple, accurate, and sensitive for rapid determination of the seven aconitum alkaloids in biological samples.

Key words: aconitum alkaloids, biological samples, consecutive reaction monitoring (CRM), liquid chromatography-linear ion trap multistage mass spectrometry (LC-LIT/MSⁿ), on-line solid phase extraction (on-line SPE)

CLC Number:

O658

ZHU Dingji, LU Minping, HUANG Kejian, ZHOU Zhe, LIN Cuiwu, YANG Ning, LIU Xiaofeng, QIAO Wentao, LI Lu, HUANG Xiaoqing. Simultaneous determination of seven aconitum alkaloids in biological samples by liquid chromatography-linear ion trap multistage mass spectrometry coupled with on-line solid phase extraction[J]. Chinese Journal of Chromatography, 2016, 34(3): 249-257.

References

[1] Qiu K, Wu H, Wang H Y. Chinese Pharmaceutical Journal, 2010, 45(8): 633 邱葵, 吴华, 王鹤尧. 中国药学杂志, 2010, 45(8): 633
[2] Wang Z Q, Jing X, Zeng R, et al. Chinese Journal of Clinical Pharmacology and Therapeutics, 2012, 17(4): 371 王志琪, 景贤, 曾嵘, 等. 中国临床药理学与治疗学, 2012, 17(4): 371
[3] Wang Z H, He Y, Zhang J Z, et al. Chinese Journal of Forensic Medicine, 2003, 18(3): 145 王朝虹, 何毅, 张继宗, 等. 中国法医学杂志, 2003, 18(3): 145
[4] Guo D, Lin J Y, Zhou C Q, et al. Strait Pharmaceutical Journal, 2011, 23(12): 32 郭丹, 林静瑜, 周春权, 等. 海峡药学, 2011, 23(12): 32
[5] Zhang X Y, Cai X X, Lin X Y, et al. Journal of Food Safety and Quality, 2013, 4(3): 715 张秀尧, 蔡欣欣, 林学尧, 等. 食品安全质量检测学报, 2013, 4(3): 715
[6] Yang C P, Liao S, Zhang T H, et al. International Journal of Pharmaceutical Research, 2012, 39(3): 256 杨翠平, 廖沙, 张天宏, 等. 国际药学研究杂志, 2012, 39(3): 256
[7] Liu J J, Li Q, Yin Y D, et al. J Sep Sci, 2014, 37(1/2): 171
[8] Zhang P P, Zhang F C, Wang Z H, et al. Chinese Journal of Chromatography, 2013, 31(3): 211 张盼盼, 张福成, 王朝虹, 等. 色谱, 2013, 31(3): 211
[9] Wu J, Shen H, Zhu L Y, et al. Chinese Journal of Hospital Pharmacy, 2011, 31(14): 1162 武洁, 沈红, 朱玲英, 等. 中国医院药学杂志, 2011, 31(14): 1162
[10] Liu W, Shen M, Wu H J, et al. Chinese Journal of Pharmaceutical Analysis, 2009, 29(12): 2023 刘伟, 沈敏, 吴何坚, 等. 药物分析杂志, 2009, 29(12): 2023
[11] Wang H L, Dong L, Xu D F, et al. Journal of Liaoning University of Traditional Chinese Medicine, 2010, 12(1): 191 王海龙, 董雷, 许大方, 等. 辽宁中医药大学学报, 2010, 12(1): 191
[12] Xiong X T, Wu H Q, Huang X L. Chinese Journal of Analytical Chemistry, 2009, 37(10): 1433 熊小婷, 吴惠勤, 黄晓兰. 分析化学, 2009, 37(10): 1433
[13] Ng S W, Ching C K, Chan A Y W, et al. J Chromatogr B, 2013, 942/943: 63
[14] Du Z X, Sun S Q. Journal of Instrumental Analysis, 2007, 26(Suppl): 61 杜振霞, 孙姝琦. 分析测试学报, 2007, 26(增刊): 61
[15] Usui K, Hayashizaki Y, Hashiyada M, et al. Leg Med, 2012, 14(3): 126
[16] Qiu P H, Chen X H, Chen X, et al. J Chromatogr B, 2008, 875(2): 471
[17] Zhang H G, Sun Y, Duan M Y, et al. Toxicon, 2005, 46(5): 500
[18] Wang Z H, Wang Z P, Wen J, et al. J Pharm Biomed Anal, 2007, 45(1): 145
[19] Hayashida M, Hayakawa H, Wada K, et al. Leg Med, 2003, 5(Suppl 1): S101
[20] Huang K J, Lu M P, Zhou Z, et al. Chinese Journal of Chromatography, 2015, 33(7): 691 黄克建, 卢敏萍, 周哲, 等. 色谱, 2015, 33(7): 691
[21] Li X, Zhang Y Q, Ai L F, et al. Chinese Journal of Chromatography, 2015, 33(6): 590 李欣, 张瑶琴, 艾连峰, 等. 色谱, 2015, 33(6): 590
[22] Duan Y S, Wang B L, Ai L F, et al. Chinese Journal of Chromatography, 2014, 32(6): 647 段永生, 王炳玲, 艾连峰, 等. 色谱, 2014, 32(6): 647
[23] Chen J, Liu Z J, An B C, et al. Chinese Journal of Chromatography, 2012, 30(10): 1068 陈静, 刘召金, 安保超, 等. 色谱, 2012, 30(10): 1068
[24] Chen J H, Lee C Y, Liau B C, et al. J Pharm Biomed Anal, 2008, 48(4): 1105
[25] US EPA. Title 40: Protection of Environment; Part 136-Guidelines Establishing Test Procedures for the Analysis of Pollutants; Appendix B to Part 136-Definition and Procedure for the Determination of the Method Detection Limit-Revision 1.11. [2015-12-21]. http://www.ecfr.gov/cgi-bin/text-idx?SID=aca7e8a173fd9625b56ff91d6a326994&mc=true&node =ap40.23.136_17.b&rgn=div9