Citation: LÜ Chen, DING Tao, MA Xin, CHEN Guosong, YUAN Fang, WU Bin, SHEN Chongyu, ZHANG Rui, FEI Xiaoqing, ZHANG Xiaoyan, CHEN Lei, LI Li. Determination of five pyrrolizidine alkaloids in honey by liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2013, 31(11): 1046-1050. doi: 10.3724/SP.J.1123.2013.06010 shu

Determination of five pyrrolizidine alkaloids in honey by liquid chromatography-tandem mass spectrometry

LÜ Chen ² ,
DING Tao ^1,, ,
MA Xin ³ ,
CHEN Guosong ² ,
YUAN Fang ¹ ,
WU Bin ¹ ,
SHEN Chongyu ¹ ,
ZHANG Rui ¹ ,
FEI Xiaoqing ¹ ,
ZHANG Xiaoyan ¹ ,
CHEN Lei ¹ ,
LI Li ⁴

1.
1. Laboratory of Food, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China;

Corresponding author: DING Tao,
Received Date: 4 June 2013
Available Online: 8 July 2013
Fund Project: 国家质检总局项目(2011IK218,2011IK209,2012IK167). (2011IK218,2011IK209,2012IK167)

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of five pyrrolizidine alkaloids (PAs) (monocrotaline, senkirkine, retrorsine, seneciphylline and senecionine) in honey. The honey samples were dissolved in 0.1 mol/L hydrochloric acid solution and a strong-cation exchange column was used to purify and concentrate the target analytes. The separation of the analytes was carried out on a Phenomenex C₁₈ column(100 mm×4.6 mm, 2.6 μm)using the mobile phases of acetonitrile and 5 mmol/L ammonium acetate-0.1% (volume percentage) formic acid aqueous solution with gradient elution. The separated compounds were detected in multiple reaction monitoring (MRM) mode via positive electrospray ionization (ESI⁺). The calibration curves were of good linearity in the range of 1-100 μg/L (r >0.99). The limit of quantification of the method was 1.0 μg/kg. The average recoveries were between 73.1% to 107.1% at three spiked levels (1, 20 and 50 μg/kg) with the relative standard deviations(RSDs)in the range of 4.1% to 17.0%. The proposed method was applied to different kinds of honey from China, New Zealand, Spain and Australia. The samples included rape, vitex, sunflower, cotton, tilia tree, date, acacia, buckwheat, manuka and eucalyptus honey. Monocrotaline, senkirkine and retrorsine were not detected in the collected honey samples. However, seneciphylline and senecionine were found in most of the honey samples. The concentrations of seneciphylline and senecionine were 11.0-31.1 μg/kg and 8.3-29.1 μg/kg, respectively.
- liquid chromatography-tandem mass spectrometry (LC-MS/MS),
- pyrrolizidine alkaloids (PAs),
- honey
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