高效液相色谱-串联质谱-PRIME HLB柱净化法测定牛乳中6 种喹诺酮残留量

doi:10.7506/rykxyjs1671-5187-20251230-093

乳业科学与技术 ›› 2026, Vol. 49 ›› Issue (3): 48-54.DOI: 10.7506/rykxyjs1671-5187-20251230-093

• 分析检测 • 上一篇

高效液相色谱-串联质谱-PRIME HLB柱净化法测定牛乳中6 种喹诺酮残留量

尹雪

辽宁省营口市农业农村综合发展服务中心,辽宁营口 115000

发布日期:2026-07-06

Determination of Six Quinolone Residues in Milk by High Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with PRIME HLB Column Purification Method

YIN Xue

An analytical method based on purification using a PRIME HLB column coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established for the simultaneous determination of six quinolone residues—ciprofloxacin, enrofloxacin, norfloxacin, sarafloxacin, ofloxacin, and pefloxacin—in bovine milk. The proposed procedure innovatively employs 0.1 mol/L ethylenediaminetetraacetic acid-Mcllvaine buffer combined with 1% formic acid-acetonitrile (2:8, V/V) as the extraction system, followed by one-step purification using a PRIME HLB column. This approach markedly simplifies conventional solid-phase extraction and reduces the sample preparation time. The purified sample was concentrated by nitrogen blowing, reconstituted, and filtered through a membrane. The separation was achieved on a C?? column (3.0 mm × 100 mm, 2.7 μm), and the HPLC-MS/MS system was operated in positive ion mode with multiple reaction monitoring. The results showed that the limits of detection for the six quinolones ranged from 0.04 to 0.10 μg/kg, and the limits of quantification from 0.13 to 0.33 μg/kg. Matrix-matched standard curves were adopted for quantification by the external standard method, which exhibited good linearity over the concentration range of 2-100 pg/L with a correlation coefficient ≥0.9961. Average recoveries from milk samples spiked at concentration levels of 2–50 μg/kg ranged from 85.5% to 106.5% with relative standard deviations ranging from 1.60% to 4.75% (n=6). This method features rapid operation, accurate results, and high precision. It provides reliable technical support for the highthroughput screening of quinolone residues in large batches of bovine milk.

Online:2026-07-06

摘要/Abstract

摘要： 建立一种结合PRIME HLB柱净化的高效液相色谱-串联质谱(high performance liquid chromatographytandem mass spectrometry,HPLC-MS/MS)法,用于同步测定牛乳中环丙沙星?恩诺沙星?诺氟沙星?沙拉沙星? 氧氟沙星和培氟沙星6 种喹诺酮类药物残留?创新性地采用0.1 mol/L乙二胺四乙酸-Mcllvaine缓冲溶液与1%甲酸乙腈溶液(2∶8,V/V)作为提取体系,并结合PRIME HLB净化柱进行一步净化,显著简化传统固相萃取操作,缩短处理时间?将净化液氮吹浓缩并复溶过膜,经C??色谱柱(3.0 mm×100 mm,2.7 μm)分离,在HPLC-MS/MS系统多反应监测模式下进行正离子扫描?结果表明,该方法对6 种喹诺酮类药物的检出限为0.04~0.10 μg/kg,定量限为 0.13~0.33 μg/kg?采用基质匹配标准曲线进行外标法定量,目标化合物在2~100 μg/L质量浓度范围内线性关系良好,相关系数≥0.9961?在牛乳样品中进行2~50 μg/kg水平的加标回收实验,平均加标回收率为85.5%~106.5%，相对标准偏差为1.60%~4.75% (n=6)?该方法操作快速?结果准确?精密度高,可为大批量牛乳中喹诺酮类残留的高通量筛查提供可靠的技术支持?

中图分类号:

TS252.7

尹雪. 高效液相色谱-串联质谱-PRIME HLB柱净化法测定牛乳中6 种喹诺酮残留量[J]. 乳业科学与技术, 2026, 49(3): 48-54 https://doi.org/10.7506/rykxyjs1671-5187-20251230-093

Agricultural and Rural Development Service Center of Yingkou City, Liaoning Province, Yingkou 115000, China. Determination of Six Quinolone Residues in Milk by High Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with PRIME HLB Column Purification Method[J]. Journal of Dairy Science and Technology, 2026, 49(3): 48-54 https://doi.org/10.7506/rykxyjs1671-5187-20251230-093

[1]	陈静，段国霞，刘丽君，吴晓莉，吕志勇，胡雪. 反相超高效液相色谱法测定乳粉中1-脱氧野尻霉素含量[J]. 乳业科学与技术, 2025, 48(6): 30-35.
[2]	曹若蕾，唐琪，张岩. 乳及乳制品中致病性微生物检测技术研究进展[J]. 乳业科学与技术, 2025, 48(6): 61-67.
[3]	屈雅莉，张彦辉，夏兆田，陈克良，周婷，楚珍珍，李飞. 分离自生牛乳的一株高产蛋白酶蜡样芽孢杆菌特性[J]. 乳业科学与技术, 2025, 48(3): 55-59.
[4]	刘璐，顾晟琳，夏亚文. 微生物法测定乳粉中VB6含量的不确定度评定[J]. 乳业科学与技术, 2025, 48(2): 30-34.
[5]	毕婷婷，魏可燕，胡明燕，田洪芸，王冠群，王文特，范丽，张海红，提静靓. 婴幼儿配方乳粉氧化机理及其过氧化值检测方法研究进展[J]. 乳业科学与技术, 2025, 48(2): 54-59.
[6]	黄建辉，张彦辉，张耀广，赵翠琴. 牛乳中β-乳球蛋白的中红外快速检测方法建立[J]. 乳业科学与技术, 2025, 48(1): 14-19.
[7]	李娇，李巧莲，周长民，袁帅，罗景阳，陈娇，丁婷. 超高效液相色谱-串联质谱法同时测定婴幼儿配方乳粉中5 种脂溶性维生素[J]. 乳业科学与技术, 2025, 48(1): 20-23.
[8]	王胜杰，梁琳. 气相色谱-质谱法测定婴幼儿配方乳粉中3-氯-1,2-丙二醇酯和缩水甘油酯[J]. 乳业科学与技术, 2024, 47(6): 31-36.
[9]	徐志鹏，泮秋立，肖晶，张爽，宋家升，王骏. 胶体金免疫层析试纸条鉴别乳品中牛、羊源性成分的性能评价[J]. 乳业科学与技术, 2024, 47(6): 37-42.
[10]	杨琦，焦昕哲，孟虎，房忠芳，张耀武，赵丽莉，张倩婷. QuEChERS处理-超高效液相色谱-串联质谱法快速检测鲜乳中54 种农药残留[J]. 乳业科学与技术, 2024, 47(6): 43-50.
[11]	白晓云，马晓冲，齐晓茹，苏运聪，张耀广，李飞. 固相萃取-气相色谱-质谱法测定牛乳中54 种农药残留[J]. 乳业科学与技术, 2024, 47(5): 12-19.
[12]	周帅康，胡连霞，王孟阳，李苗，卢涵，王世杰. 基于实时荧光定量环介导等温扩增技术快速检测发酵乳中嗜热链球菌和保加利亚乳杆菌[J]. 乳业科学与技术, 2024, 47(3): 9-15.
[13]	梁建英，唐烁，刘丽君，黄晓燕，岳虹，胡文慧，李翠枝. 乳及乳制品中蛋白酶检测技术研究进展[J]. 乳业科学与技术, 2024, 47(3): 80-85.
[14]	祁兵，陈柔含，杨晓君，江春铃，马颖清，邓波. 基于生物芯片技术的生乳中兽药检测方法验证及其应用[J]. 乳业科学与技术, 2024, 47(2): 42-48.
[15]	刘予煊，孟根花，蔺婷娟，郭瑞芳. 婴幼儿配方乳粉中1,2-丙二醇检测方法的优化[J]. 乳业科学与技术, 2024, 47(2): 49-55.

高效液相色谱-串联质谱-PRIME HLB柱净化法测定牛乳中6 种喹诺酮残留量

Determination of Six Quinolone Residues in Milk by High Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with PRIME HLB Column Purification Method

RichHTML

PDF (PC)

可视化

摘要/Abstract

引用本文

使用本文

参考文献

相关文章 15

编辑推荐

Metrics