通过式固相萃取-超高效液相色谱-串联质谱法测定水产品中多种氟喹诺酮类和苯二氮?类药物-食品安全质量检测学报-CSCIED科技核心评价数据库-手机版

通过式固相萃取-超高效液相色谱-串联质谱法测定水产品中多种氟喹诺酮类和苯二氮?类药物

Determination of multiple fluoroquinolones and benzodiazepines in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry with pass-through solid phase extraction

ES评分 0 浏览量：186 下载量：0

全文阅读下载引用收藏

DOI	10.19812/j.cnki.jfsq11-5956/ts.20250409008
刊名	食品安全质量检测学报 Journal of Food Safety and Quality
年，卷(期)	2025, 16(13)
作者	王鼎南, 吴新雅, 李诗言, 周钦, 柯庆青, 张宜明, 王扬*,
作者单位	浙江省水产技术推广总站; 浙江农林大学食品与健康学院
摘要	目的建立一种超高效液相色谱-串联质谱法(ultra-performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定水产品中6种氟喹诺酮类和4种苯二氮?类药物残留的分析方法。方法使用1%甲酸乙腈溶液对水产样品进行提取, 提取液经旋转蒸发仪浓缩后用90%乙腈水溶液(含1%甲酸)复溶, 经通过式固相萃取小柱(ProElut PLS-A)净化后直接供UPLC-MS/MS分析, 采用同位素内标法进行定量。结果 10种目标化合物在0.5~50.0 ng/mL质量浓度范围内线性关系良好, 相关系数(r)均大于0.998。10种目标化合物在5种水产品基质中定量限为0.5~1.0 μg/kg, 低、中、高3个不同水平的加标回收率范围为81.5%~109.7%, 相对标准偏差为0.24%~13.22%。结论经方法学验证, 该方法灵敏度高、定量准确、稳定性好、操作简单高效, 可用于水产品中6种氟喹诺酮类和4种苯二氮?类药物残留的高通量检测。
Abstract	Objective To establish an analytical method for the simultaneous determination of 6 kinds of fluoroquinolones and 4 kinds of benzodiazepines residues in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Aquatic product samples were extracted with 1% formic acid in acetonitrile. The extracts were concentrated with a rotary evaporator and then reconstituted in 90% acetonitrile aqueous solution (containing 1% formic acid), and purified through a pass-through solid phase extraction cartridge (ProElut PLS-A). The purified extracts were directly analyzed by UPLC-MS/MS. Quantification was performed using the isotope internal standard method. Results The 10 kinds of target compounds exhibited good linearity within the concentration range of 0.5 to 50.0 ng/mL, with correlation coefficients (r) all greater than 0.998. The limits of quantitation for these compounds in 5 kinds of different aquatic product matrices ranged from 0.5 to 1.0 μg/kg. The recovery rates at low, medium and high spiking levels ranged from 81.5% to 109.7%, with relative standard deviations ranging from 0.24% to 13.22%. Conclusion Methodological validation confirmed that the developed method is highly sensitive, accurate in quantification, stable, and straightforward in operation. It is suitable for high-throughput detection of 6 kinds of fluoroquinolones and 4 kinds of benzodiazepines residues in aquatic products.
关键词	氟喹诺酮，苯二氮卓，水产品，通过式固相萃取
KeyWord	fluoroquinolones; benzodiazepines; aquatic products; pass-through solid phase extraction
基金项目
页码	26-36

参考文献
相关文献

[1] 农业农村部渔业渔政管理局, 全国水产技术推广总站, 中国水产学会. 2024 中国渔业统计年鉴
[M]. 北京: 中国农业出版社, 2024. Fishery and Fishery Administration Bureau of the Ministry of Agriculture and Rural Affairs, National Fisheries Technology Extension Center, China Society of Fisheries. China fishery statistical yearbook 2024
[M]. Beijing: China Agriculture Press, 2024.
[2] 高宏泉, 高翔, 陈家勇. 2024年全国渔业经济形势分析
[J]. 中国渔业经济, 2025, 43(1): 2–8, 81. GAO HQ, GAO X, CHEN JY. Analysis of the national fishery economic situation in 2024
[J]. Chinese Fisheries Economics, 2025, 43(1): 2–8, 81.
[3] 张海琪, 高令梅. 共同富裕背景下浙江渔业高质量发展对策研究
[J]. 中国渔业经济, 2024, 42(6): 37–45. ZHANG HQ, GAO LM. Study on countermeasures for the high-quality development of Zhejiang fisheries
[J]. Chinese Fisheries Economics, 2024, 42(6): 37–45.
[4] 张钦, 冉瑞玲, 易良键, 等. 水产品食用品质特征研究进展
[J]. 食品安全导刊, 2024(19): 136–139. ZHANG Q, RAN RL, YI LJ, et al. Research progress on edible quality characteristics of aquatic products
[J]. China Food Safety Magazine, 2024(19): 136–139.
[5] 陈莉, 李太平. 2019—2020 年沿海与内陆地区水产品质量安全比较研究
[J]. 中国渔业质量与标准, 2022, 12(2): 60–66. CHEN L, LI TP. Study on quality and safety comparison of aquatic products in China’s coastal and inland areas from 2019 to 2020
[J]. Chinese Fishery Quality and Standards, 2022, 12(2): 60–66.
[6] SAXENA N, SHANKHDHAR S, KUMAR A, et al. Part 2, studies on the synthesis of quinolone derivatives with their biological activity
[J]. Current Organic Chemistry, 2024, 28(3): 185–212.
[7] BUSH NG, DIEZ-SANTOS I, KRISHNA PS, et al. Insights into antibiotic resistance promoted by quinolone exposure
[J]. Antimicrobial Agents and Chemotherapy, 2025, 69(1): e00997-24.
[8] YI B, BIN L, YANG L, et al. Research advances of detection methods for quinolones residues in foods
[J]. Chinese Journal of Analytical Chemistry, 2022, 50(10): 1444–1455.
[9] LI SY, CHEN Z, HUANG L, et al. Safety of quinolones in children: A systematic review and meta-analysis
[J]. Pediatric Drugs, 2022, 24(5): 447–464.
[10] LOPEZ AL, BUIL PO, BANZO MJA. Severe quinolone-induced hypoglycemia
[J]. Medicina Clinica, 2023, 161(5): 229.
[11] ENGIN E. GABAA receptor subtypes and benzodiazepine use, misuse, and abuse
[J]. Frontiers in Psychiatry, 2023, 13: 1–14.
[12] BERRO LF, FIDALGO TM, ROWLETT JK, et al. Benzodiazepine addiction: From lab to street
[J]. Frontiers in Psychiatry, 2023, 14: 1–7.
[13] HUFF C, FINLAYSON AJR, FOSTER DE, et al. Enduring neurological sequelae of benzodiazepine use: An Internet survey
[J]. Therapeutic Advances in Psychopharmacology, 2023, 13: 1–9.
[14] WU RB, RUAN YF, LIN HJ, et al. Occurrence and fate of psychiatric pharmaceuticals in wastewater treatment plants in Hong Kong: Enantiomeric profiling and preliminary risk assessment
[J]. Acs Es & T Water, 2020, 1(3): 542–552.
[15] LFFLER D, RMBKE J, MELLER M, et al. Environmental fate of pharmaceuticals in water/sediment systems
[J]. Environmental Science & Technology, 2005, 39(14): 5209–5218.
[16] BRAND JA, BERTRAM MG, CERVENY D, et al. Psychoactive pollutant alters movement dynamics of fish in a natural lake system
[J]. Proceedings of the Royal Society B-Biological Sciences, 2024, 291: 1–12.
[17] SHAN Q, HUANG XS, YE SC, et al. Residue behavior and risk assessment of diazepam and its metabolites in crucian carp (Carassius auratus) after oral administration
[J]. Journal of Veterinary Pharmacology and Therapeutics, 2025, 1: 1–9.
[18] 贝亦江, 周钦, 周以琳, 等. 2018—2019年浙江省养殖水产品中6种喹诺酮类药物残留分析及风险评估
[J]. 食品安全质量检测学报, 2021, 12(5): 2011–2017. BEI YJ, ZHOU Q, ZHOU YL, et al. Analysis and risk assessment of 6 quinolones residues in aquatic products in Zhejiang Province from 2018 to 2019
[J]. Journal of Food Safety & Quality, 2021, 12(5): 2011–2017.
[19] 欧阳萍, 王军淋, 张念华, 等. 通过式固相萃取净化结合超高效液相色谱-串联质谱法测定鱼肉中地西泮及 3 种代谢物
[J]. 卫生研究, 2025, 54(1): 129–135. OUYANG P, WANG JL, ZHANG NH, et al. Determination of diazepam and its three metabolites in fish by pass-through solid phase extraction purification combined with ultra performance liquid chromatography- tandem mass spectrometry
[J]. Journal of Hygiene Research, 2025, 54(1): 129–135.
[20] PAN YT, YANG HJ, WEN K. Current advances in immunoassays for quinolones in food and environmental samples
[J]. Trac-Trends in Analytical Chemistry, 2022, 157: 1–18.
[21] WANG J, WANG YL, PAN YH, et al. Preparation of a broadly specific monoclonal antibody-based indirect competitive ELISA for the detection of benzodiazepines in edible animal tissues and feed
[J]. Food Analytical Methods, 2016, 9(12): 3407–3419.
[22] LI HF, YIN JG, LIU YM, et al. Effect of protein on the detection of fluoroquinolone residues in fish meat
[J]. Journal Agricultural and Food Chemistry, 2012, 60(7): 1722–1727.
[23] VARDINI MT, MASHAYEKHI HA, SABER-TEHRANI M, et al. Dispersive liquid-liquid microextraction followed by high-performance liquid chromatography as an efficient and sensitive technique for the simultaneous determination of alprazolam, oxazepam, and diazepam in human urine samples
[J]. Journal of Liquid Chromatography & Related Technologies, 2012, 35(7): 988–999.
[24] 刘书余. 禽肉、猪肉和禽蛋中4种氟喹诺酮类药物残留气相色谱-串联质谱检测方法的研究
[D]. 扬州: 扬州大学, 2024. LIU SY. Study on four fluoroquinolones in poultry meat, pork and poultry eggs by gas chromatography-tandem mass spectrometry detection method
[D]. Yangzhou: Yangzhou University, 2024.
[25] VLAD CS, DUMITRASCU V, VLAD DC, et al. Fast and simple method for simultaneous detection and quantification of diazepam and desmethyldiazepam in plasma samples in psychiatric patients by GC-MS-FID
[J]. Revista De Chimie, 2017, 68(3): 530–533.
[26] 魏丹, 国明, 张菊. 加速溶剂萃取-磁固相萃取-高效液相色谱-串联质谱法测定水产品中10 种氟喹诺酮类药物残留
[J]. 色谱, 2020, 38(12): 1413–1422. WEI D, GUO M, ZHANG J. Determination of 10 fluoroquinolones residues in aquatic products by accelerated solvent extraction, magnetic solid-phase extraction, and high performance liquid chromatography- tandem mass spectrometry
[J]. Chinese Journal of Chromatography, 2020, 38(12): 1413–1422.
[27] 孙雷, 张骊, 徐倩, 等. 超高效液相色谱-串联质谱法检测猪肉和猪肾中残留的10种镇静剂类药物
[J]. 色谱, 2010, 28(1): 38–42. SUN L, ZHANG L, XU Q, et al. Determination of ten sedative residues in pork and kidney by ultra performance liquid chromatography-tandem mass spectrometry
[J]. Chinese Journal of Chromatography, 2010, 28(1): 38–42.
[28] TSAI CW, LIN CS, WANG WH, et al. Multi-residue determination of sulfonamide and quinolone residues in fish tissues by high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS)
[J]. Journal of Food and Drug Analysis, 2012, 20(3): 674–680.
[29] 陈兴连, 林涛, 刘兴勇, 等. 超高效液相色谱-串联质谱法快速测定鱼和虾中多类禁、限用兽药残留
[J]. 色谱, 2020, 38(5): 538–546. CHEN XL, LIN T, LIU XY, et al. Rapid determination of multiple prohibited and restricted veterinary drug residues in fish and shrimp by ultra performance liquid chromatography-tandem mass spectrometry
[J]. Chinese Journal of Chromatography, 2020, 38(5): 538–546.
[30] 魏玉霞, 王芳, 左郡, 等. QuEChERS-超高效液相色谱-串联质谱法同时测定淡水鱼和淡水虾中的11种喹诺酮类兽药残留量
[J]. 食品安全质量检测学报, 2021, 12(7): 2906–2912. WEI YX, WANG F, ZUO J, Simultaneous determination of 11 quinolone residues in fresh water fish and shrimp by QuEChERS purification coupled with ultra performance liquid chromatography-tandem mass spectrometry
[J]. Journal of Food Safety & Quality, 2021, 12(7): 2906–2912.
[31] 邹游, 邵琳智, 陈思敏, 等. QuEChERS-高效液相色谱-串联质谱法测定动物源性食品中3种镇静剂残留
[J]. 色谱, 2017, 35(8): 801–807. ZOU Y, SHAO LZ, CHEN SM, et al. Determination of three tranquillizer residues in animal foods by QuEChERS-high performance liquid chromatography-tandem mass spectrometry
[J]. Chinese Journal of Chromatography, 2017, 35(8): 801–807.
[32] TANG YY, LU HF, LIN HY, et al. Development of a quantitative multi-class method for 18 antibiotics in chicken, pig, and fish muscleusing UPLC-MS/MS
[J]. Food Analytical Methods, 2012, 5(6): 1459–1468.
[33] 苏焕斌, 王思琦, 毛云枫, 等. 超高效液相色谱串联质谱法检测水产品中的地西泮残留
[J]. 食品安全导刊, 2024(35): 64–68. SU HB, WANG SQ, MAO YF, et al. Detection of diazepam residues in aquatic products by ultra high performance liquid chromatography tandem mass spectrometry
[J]. China Food Safety Magazine, 2024(35): 64–68.
[34] 孙晓杰, 高金芳, 李兆新, 等. 通过式净化-液相色谱-串联质谱快速筛查水产品中15类107种兽药多残留的方法研究
[J]. 食品安全质量检测学报, 2020, 11(22): 8240–8246. SUN XJ, GAO JF, LI ZX, et al. Simultaneous determination of 15 categories and 107 kinds of veterinary drugs in aquatic products by pass-through purification and liquid chromatography-tandem mass spectrometry
[J]. Journal of Food Safety & Quality, 2020, 11(22): 8240–8246.
[35] 何连军, 王鼎南, 张宜明, 等. 通过型固相萃取-高效液相色谱-串联质谱法同时测定水产品中的5种硝基咪唑和地西泮
[J]. 核农学报, 2021, 35(8): 1865–1874. nitroimidazoles HE LJ, WANG DN, ZHANG YM, et al. Simultaneous determination of five and diazepam in aquatic products by high-performance liquid chromatography-tandem mass spectrometry with pass-through solid phase extraction purification
[J]. Journal of Nuclear Agricultural Sciences, 2021, 35(8): 1865–1874.
[36] 李诗言, 柯庆青, 王鼎南, 等. PRIME HLB固相萃取-超高效液相色谱串联质谱法同时测定水产品中11种酰胺醇和抗病毒类药物残留
[J]. 分析试验室, 2023, 42(4): 514–520. LI SY, KE QQ, WANG DN, et al. Simultaneous determination of eleven amphenicols and antiviral drugs in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry coupled with PRIME HLB solid phase extraction
[J]. Chinese Journal of Analysis Laboratory, 2023, 42(4): 514–520.
[37] 王旭峰, 王强, 张英侠, 等. 固相萃取净化/超高效液相色谱-串联质谱法测定养殖环境中地西泮及其代谢物
[J]. 分析测试学报, 2023, 42(3): 337–343. WANG XF, WANG Q, ZHANG YX, et al. Determination of diazepam and its metabolites in aquaculture environment samples by solid phase extraction cleanup and ultra performance liquid chromatography-tandem mass spectrometry
[J]. Journal of Instrumental Analysis, 2023, 42(3): 337–343.
[38] 宿书芳, 孙立臻, 薛霞, 等. 通过式固相萃取-超高效液相色谱-串联质谱法测定水产品中地西泮
[J]. 色谱, 2020, 38(7): 791–797. SU SF, SUN LZ, XUE X, et al. Determination of diazepam in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry with pass-through solid phase extraction
[J]. Chinese Journal of Chromatography, 2020, 38(7): 791–797.
[39] 杨文珺, 王华. 液相色谱串联质谱法测定猪肉中的兽药残留
[J]. 食品安全导刊, 2025(5): 106–109. YANG WJ, WANG H. Determination of veterinary drug residues in pork by liquid chromatography-tandem mass spectrometry
[J]. China Food Safety Magazine, 2025(5): 106–109.
[40] 孔祥一, 庄丽丽, 方恩华, 等. QuEChERS-同位素稀释-气相色谱-串联质谱法测定动物源性食品中 9 种 N-亚硝胺类化合物
[J]. 色谱, 2021, 39(1): 96–103. KONG XY, ZHANG LL, FANG ENH, et al. Determination of nine N-nitrosamines in animal-derived foods by QuEChERS-isotope dilution combined with gas chromatography-tandem mass spectrometry
[J]. Chinese Journal of Chromatography, 2021, 39(1): 96–103.
[41] 林涛, 蔡苇, 王志飞, 等. 高效液相色谱-质谱法测定淡水鱼中地西泮
[J]. 化学分析计量, 2024, 33(9): 28–32. LIN T, CAI W, WANG ZF, et al. Determination of diazepam in freshwater fish by high performance liquid chromatography mass spectrometry
[J]. Chemical Analysis and Meterage, 2024, 33(9): 28–32.

引用本文

王鼎南, 吴新雅, 李诗言, 周钦, 柯庆青, 张宜明, 王扬*. 通过式固相萃取-超高效液相色谱-串联质谱法测定水产品中多种氟喹诺酮类和苯二氮?类药物 [J]. 食品安全质量检测学报. 2025; 16; (13). 26 - 36.

文献评论

相关学者

相关机构