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Citation: ZHANG Xiaoguang, LIU Dong, LIU Hongran, LI Qiang, LI Lili, WANG Lixia, ZHANG Yan. Liquid chromatography-tandem mass spectrometry method for determination of 10 macrolide antibiotics in pork samples using on-line solid phase extraction purification[J]. Chinese Journal of Chromatography, ;2017, 35(10): 1055-1061. doi: 10.3724/SP.J.1123.2017.04004 shu

Liquid chromatography-tandem mass spectrometry method for determination of 10 macrolide antibiotics in pork samples using on-line solid phase extraction purification

ZHANG Xiaoguang ^1, ,
LIU Dong ¹ ,
LIU Hongran ¹ ,
LI Qiang ¹ ,
LI Lili ² ,
WANG Lixia ¹ ,
ZHANG Yan ¹

1.
Hebei Food Inspection and Research Institute, Key Laboratory of Food Safety of Hebei Province, Shijiazhuang 050091, China;
2.
Shijiazhuang Food and Drug Inspection Institute, Shijiazhuang 050011, China

Received Date: 5 April 2017

Fund Project: National Science and Technology Support Program (No. 2015BAK36B03)

A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method based on-line solid phase extraction (SPE) purification was established to determine 10 macrolide antibiotics in pork samples. The samples were extracted with acetonitrile, and the extracts were dried with rotary evaporator at 40℃, then the analytes were dissolved with 2 mL phosphate buffer. The solutions were purified and concentrated by on-line SPE with HLB cartridges. The analytes were eluted with methanol, and then transferred to XBridge BEH C18 column, separated with the mobile phases of 10 mmol/L ammonium acetate aqueous solution and acetonitrile. Finally, the target analytes were detected by tandem mass spectrometry. The results showed that good linearity was obtained in the range of 0.1-200 μg/L for the 10 macrolide antibiotics with correlation coefficients better than 0.990. The limits of detection were in range of 0.05-0.30 μg/kg and the limits of quantitation were in range of 0.10-1.00 μg/kg. The recoveries of the method were in range of 69.6%-115.2% at the spiked levels of 0.10-10.0 μg/kg for all analytes, with the relative standard deviations less than 10%. The developed method can be used for the determination of the 10 macrolide antibiotics in pork samples.
- on-line solid phase extraction (SPE),
- liquid chromatography-tandem mass spectrometry (LC-MS/MS),
- macrolide antibiotics,
- pork
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