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| Determination of Nine Kinds of Sulfonamides Residues in Gizzard Pepsin by Ultra-performance Liquid Chromatography－Tandem Mass Spectrometry |
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| DOI： |
| KeyWord:Gizzard Pepsin sulfonamides ultra-performance liquid chromatography－tandem mass spectrometry QuEChERS PRiME HLB |
| Author | Institution |
| XU Xiao-hui，WANG Xiao-qiao，DONG Wei，WU Fu-xiang，DU Rui-hu，ZHU Ren-yuan，SHI Xiao-feng |
1. Lanzhou Institute for Food and Drug Control， Lanzhou ， China; 2. Gansu Provincial Academic Institute for Medical Research， Lanzhou ， China; 3. Lanzhou Zhongjianke Testing Technology Co.， Ltd， Lanzhou ， China |
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| Abstract: |
| In order to evaluate the risk of sulfonamides residues in Gizzard Pepsin， a comprehensive analytical method was developed for the qualitative and quantitative determination of nine kinds of sulfonamides in Gizzard Pepsin by ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry（UPLC－MS/MS） in this paper.The sample was extracted by QuEChERS with ultrasonic method，then purified with PRiME HLB．The chromatographic separation was performed on an ACQUITY BEH C18 chromatographic column（2.1 mm × 100 mm，1.7 μm），with 0.1% formic acid－2 mmol/L ammonium acetate aqueous solution and acetonitrile containing 0.1% formic acid as mobile phases by gradient elution.The analytes were detected by electrospray ionization mass spectrometry in positive mode under dynamic multiple reaction monitoring（d－MRM） mode，and quantified by external standard method．Results showed that the nine sulfonamides showed good linearities in the concentration range of 0－50 ng/mL with their correlation coefficients（r2） not less than 0.996 0．The limits of detection（LOD，S/N = 3） and limits of quantitation（LOQ，S/N = 10） were in the ranges of 0.065 4－0.715 7 μg/kg and 0.212 2－2.478 μg/kg，respectively.The recoveries for the analytes at three spiked levels were in the range of 63.2%－88.7%，with relative standard deviations（RSD） of 0.90%－7.1%．The developed method was simple，rapid and accurate，and was applied to the detection on 10 batches of Gizzard Pepsin samples，among which one was found to contain sulfamethoxazole residue． |
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