Citation: LEI Meikang, PENG Fang, DING Tao, ZHU Zitong, XU Jiawen, WU Xiaoqin. Determination of wilforine in honey using solid phase extraction purification and ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2015, 33(1): 65-67. doi: 10.3724/SP.J.1123.2014.08022 shu

Determination of wilforine in honey using solid phase extraction purification and ultra performance liquid chromatography-tandem mass spectrometry

LEI Meikang ^1,, ,
PENG Fang ¹ ,
DING Tao ² ,
ZHU Zitong ¹ ,
XU Jiawen ¹ ,
WU Xiaoqin ¹

1.
1. Technology Center of Quzhou Entry-Exit Inspection and Quarantine Bureau, Quzhou 324002, China;

Corresponding author: LEI Meikang,
Received Date: 22 August 2014
Available Online: 23 September 2014
Fund Project: 浙江省公益性技术应用研究计划项目(2013C37101). (2013C37101)

A method based on solid phase extraction and ultra performance liquid chromatography coupled with tandem mass spectrometry (SPE-UPLC-MS/MS) has been proposed for the determination of wilforine residue in honey. After the sample was dissolved with water, concentrated and purified by an HLB solid phase extraction cartridge, the UPLC separation was performed on a Hypersil GOLD C18 column (50 mm ×2.1 mm, 1.9 μm) utilizing a gradient elution program of methanol (containing 0.15% formic acid) and water as mobile phases at a flow rate of 0.25 mL/min. The determination was carried out with electrospray ion source in the positive mode (ESI⁺) and multiple reaction monitoring (MRM) mode. The mass concentration of wilforine in the range of 0.01-2 μg/L was linearly correlated with the peak area, and the correlation coefficients was greater than 0.998. The limit of quantification (S/N>10) for wilforine was 0.01 μg/kg. The recoveries were 76.1% to 96.2% in the spiked levels of 0.01, 0.05 and 0.5 μg/kg with the relative standard deviations (RSD, n=6) lower than 10%. The results indicate that the method is rapid, sensitive and accurate, and can be applied for the qualitative and quantitative analysis of wilforine in honey.
- solid phase extraction (SPE),
- ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS),
- wilforine,
- honey
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