Determination of 25 Glucocorticoids in Milk by Ultra-performance Liquid Chromatography - Tandem Mass Spectrometry with Nanofiber Solid Phase Extraction

WU Xiao-xiao; JIANG Di-yao; MEI Xiu-ming; KANG Xue-jun; LI Yu-feng; ZHANG Chi

doi:10.19969/j.fxcsxb.22022805

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Determination of 25 Glucocorticoids in Milk by Ultra-performance Liquid Chromatography - Tandem Mass Spectrometry with Nanofiber Solid Phase Extraction

Scientific Papers | 更新时间：2022-06-22

- Determination of 25 Glucocorticoids in Milk by Ultra-performance Liquid Chromatography - Tandem Mass Spectrometry with Nanofiber Solid Phase Extraction
- Journal of Instrumental Analysis Vol. 41, Issue 6, Pages: 812-819(2022)
- 作者机构：
  
  1.南京市产品质量监督检验院国家市场监管重点实验室（生物毒素分析与评价），江苏南京 210019
  2.东南大学生物科学与医学工程学院，江苏南京 210096
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.22022805
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吴肖肖,蒋迪尧,梅秀明等.纳米纤维固相萃取/超高效液相色谱-串联质谱法检测牛奶中25种糖皮质激素[J].分析测试学报,2022,41(06):812-819.

WU Xiao-xiao,JIANG Di-yao,MEI Xiu-ming,et al.Determination of 25 Glucocorticoids in Milk by Ultra-performance Liquid Chromatography - Tandem Mass Spectrometry with Nanofiber Solid Phase Extraction[J].Journal of Instrumental Analysis,2022,41(06):812-819.
吴肖肖,蒋迪尧,梅秀明等.纳米纤维固相萃取/超高效液相色谱-串联质谱法检测牛奶中25种糖皮质激素[J].分析测试学报,2022,41(06):812-819. DOI： 10.19969/j.fxcsxb.22022805.

WU Xiao-xiao,JIANG Di-yao,MEI Xiu-ming,et al.Determination of 25 Glucocorticoids in Milk by Ultra-performance Liquid Chromatography - Tandem Mass Spectrometry with Nanofiber Solid Phase Extraction[J].Journal of Instrumental Analysis,2022,41(06):812-819. DOI： 10.19969/j.fxcsxb.22022805.

摘要

采用静电纺丝技术制备了聚苯乙烯（PS）纳米纤维，用扫描电镜、透射电镜和红外光谱对其进行表征，并测试了比表面积和接触角。经过色谱条件、萃取条件优化，建立了基于纳米纤维固相萃取前处理/超高效液相色谱 - 串联质谱检测牛奶中25种糖皮质激素类药物残留的分析方法。样品经乙腈振荡提取，PS纳米纤维固相萃取柱富集净化，甲醇洗脱液用ACQUITY BEH C,18,（2.1 mm × 100 mm，1.7 μm）分离，以0.1%甲酸水 - 乙腈为流动相进行梯度洗脱，在双喷射流电喷雾正离子模式下，以多反应监测模式（MRM）进行检测，外标法定量。结果表明，25种糖皮质激素在1~100 µg/L范围内线性关系良好，相关系数（,r,）均大于0.995，方法检出限（LOD，,S,/,N, ≥ 3）和定量下限（LOQ，,S,/,N, ≥ 10）分别为0.04 ~ 0.10 µg/kg和0.13 ~ 0.33 μg/kg。在3个不同浓度加标水平下，25种糖皮质激素的回收率为71.5% ~ 105%，相对标准偏差（RSD）为1.8% ~ 10%。该方法操作简单、快速、准确、灵敏度高，应用该方法检测10批牛奶样品，有1批次检出微量氢化可的松残留。

Abstract

A novel ultra-performance liquid chromatography - tandem mass spectrometry（UPLC - MS/MS） with polystyrene（PS） nanofiber solid phase extraction was developed for the simultaneous determination of 25 glucocorticoids in milk after the optimization of chromatographic and extraction conditions. The PS nanofiber was prepared by electrostatic spinning，then characterized by scanning electron microscopy， transmission electron microscopy and infrared spectroscopy. Subsequently， the BET surface area and contact angle of the PS nanofiber were measured. The milk sample was extracted using vortex mixer with acetonitrile. The analytes were concentrated and purified with the PS nanofiber solid phase extraction column. The chromatographic separation of the methanol eluent was performed on an ACQUITY BEH C,18 ,（2.1 mm × 100 mm，1.7 μm） column by gradient elution，with 0.1% formic acid aqueous solution and acetonitrile as mobile phases. The analysis was performed by mass spectrometry with jet stream electrospray ionization in positive mode under multiple reaction monitoring（MRM） mode. The analytes were quantified by external standard method. Results of the method validation showed that there were good linear relationships for 25 glucocorticoids in the concentration range of 1 - 100 µg/L，with their correlation coefficients（,r,） larger than 0.995.The limits of detection（LOD，,S,/,N, ≥ 3） and limits of quantitation（LOQ，,S,/,N, ≥ 10） for 25 glucocorticoids were in the range of 0.04 - 0.10 µg/kg and 0.13 - 0.33 μg/kg，respectively. The recoveries for 25 glucocorticoids in the spiked sample at three concentration levels ranged from 71.5% to 105%，with relative standard deviations（RSDs） of 1.8% - 10%. The established method is simple，rapid，accurate and sensitive. The method was applied to detect 25 glucocorticoids in 10 batches of milk samples. Only one of them were found to contain trace hydrocortisone residue.

关键词

糖皮质激素纳米纤维固相萃取聚苯乙烯超高效液相色谱 - 串联质谱法牛奶

Keywords

glucocorticoidsnanofiber solid phase extractionpolystyreneultra-performance liquid chromatography - tandem mass spectrometrymilk

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