Citation: 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. doi: 10.3724/SP.J.1123.2015.10044 shu

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

ZHU Dingji ¹ ,
LU Minping ² ,
HUANG Kejian ^3,, ,
ZHOU Zhe ⁴ ,
LIN Cuiwu ² ,
YANG Ning ³ ,
LIU Xiaofeng ³ ,
QIAO Wentao ³ ,
LI Lu ³ ,
HUANG Xiaoqing ³

1.
1. Guangxi Zhuang Autonomous Region Academy for the Prevention and Treatment of Occupational Diseases, Nanning 530021, China;
2.
2. School of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004, China;
3.
3. Evidence Identification Center, Guangxi Zhuang Autonomous Region Public Security Department, Nanning 530012, China;
4.
4. Thermo Fisher Scientific (China) Co., Ltd., Shanghai 201206, China

Corresponding author: HUANG Kejian,
Received Date: 29 October 2015

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.
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