磁分散固相萃取结合LC⁃MS/MS分析鱼肌肉中16种麻醉剂残留量

doi:10.3969/j.issn.1004-1524.20250048

浙江农业学报 ›› 2026, Vol. 38 ›› Issue (1): 148-159.DOI: 10.3969/j.issn.1004-1524.20250048

磁分散固相萃取结合LC⁃MS/MS分析鱼肌肉中16种麻醉剂残留量

王美玉¹^,²(), 刘真真², 王新全², 王娇², 刘小琦¹^,², 谷晨舒¹^,², 杜丽慧¹^,^*(), 齐沛沛¹^,²^,^*()

1.宁波大学食品科学与工程学院,农产品质量安全全国重点实验室,浙江宁波 315832
2.浙江省农业科学院农产品质量安全与营养研究所,农产品质量安全全国重点实验室,浙江杭州 310021

收稿日期:2025-01-20 出版日期:2026-01-25 发布日期:2026-02-11
作者简介:齐沛沛,E-mail:qipeipei@zaas.ac.cn
*杜丽慧,E-mail:dulihui@nbu.edu.cn;
王美玉,研究方向为食品加工与安全。E-mail:wmy2156114686@163.com
通讯作者: 杜丽慧,齐沛沛
基金资助:
浙江省重点研发计划(2023C02038);浙江省重点研发计划(2020C02023)

Determination of 16 anesthetic residues in fish muscle by magnetic dispersive solid-phase extraction combined with LC-MS/MS

WANG Meiyu¹^,²(), LIU Zhenzhen², WANG Xinquan², WANG Jiao², LIU Xiaoqi¹^,², GU Chenshu¹^,², DU Lihui¹^,^*(), QI Peipei¹^,²^,^*()

1. School of Food Science and Engineering, State Key Laboratory for Quality and Safety of Agro-Products, Ningbo University, Ningbo 315832, Zhejiang, China
2. Institute of Agro-Product Safety and Nutrition, State Key Laboratory for Quality and Safety of Agro-Products, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China

Received:2025-01-20 Online:2026-01-25 Published:2026-02-11
Contact: DU Lihui,QI Peipei

摘要/Abstract

摘要：

为建立鱼肌肉中16种麻醉剂残留的同步检测方法,本研究以磁性纳米材料为净化吸附剂,基于QuEChERS前处理技术,结合液相色谱-串联质谱(LC-MS/MS)建立了鱼肌肉中卡因类、苯二氮卓类和吩噻嗪类麻醉剂的检测方法。优化了萃取溶剂类型、磁性纳米材料Fe₃O₄@SiO₂@DVB-NVP(聚二乙烯基苯-吡咯烷酮,Fe₃O₄-PLS)和N-丙基乙二胺(PSA)用量对目标物回收率的影响。确定以含0.5%(体积分数)乙酸的乙腈为萃取剂,氯化钠(NaCl)和无水硫酸镁(MgSO₄)为盐析与除水材料,20 mg Fe₃O₄-PLS、10 mg PSA为净化吸附材料。在正离子电喷雾模式下,采用Luna Omega C₁₈色谱柱(100 mm×2.1 mm,1.6 μm)分离,外标法定量。结果表明,16种麻醉剂在0.5~200 μg·kg^-1范围内线性关系良好,相关系数(r)≥ 0.996,仪器检出限(limit of detection, LOD)为0.08~0.57 μg·L^-1。在1、10、100 μg·kg^-1的添加水平下,16种麻醉剂的平均加标回收率为72.4%~110.8%,日内相对标准偏差(relative standard deviation, RSD)为0.4%~7.7%。实际样品分析中,三卡因和苯佐卡因检出率分别为26.1%和39.1%,二者的检出质量分数范围分别为2.07~6.34 μg·kg^-1和1.44~2.87 μg·kg^-1。本方法实用性强,可为鱼肌肉中16种麻醉剂的高通量残留分析提供参考。

关键词: 磁性纳米材料, 液相色谱-串联质谱, 麻醉剂, 鱼

Abstract:

To establish a simultaneous determination method for 16 anesthetic residues in fish muscle, a detection method for caine-type, benzodiazepines, and phenothiazine anesthetics in fish muscle was developed based on a QuEChERS pretreatment technique using magnetic nanomaterials as clean-up adsorbents, combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS). The effects of extraction solvent type, the dosage of magnetic nanomaterial Fe₃O₄@SiO₂@DVB-NVP(polyvinylphenylpyrrolidone, Fe₃O₄-PLS) and N-propylethylenediamine(PSA) on the recovery rate of the target substance were optimized. It was determined that 0.5%(volume fraction) acetic acid in acetonitrile was used as the extractant, sodium chloride (NaCl) and anhydrous magnesium sulfate (MgSO₄) were used as the salting out and water removal materials, and 20 mg Fe₃O₄-PLS and 10 mg PSA were used as the purification and adsorption materials. In the positive ion electrospray mode, the Luna Omega C₁₈ chromatographic column(100 mm×2.1 mm, 1.6 μm) was used for separation and quantification by the external standard method. The results showed that the 16 anesthetics had good linearity within the range of 0.5 to 200 μg·kg^-1, with correlation coefficient(r) ≥ 0.996, and the limit of detection(LOD) of the instrument was 0.08-0.57 μg·L^-1. At the addition levels of 1, 10, and 100 μg·kg^-1, the average spiked recovery rates of the 16 anesthetics ranged from 72.4% to 110.8%, with intra-day relative standard deviation (RSD) of 0.4%-7.7%. In the analysis of real samples, the detection rates for tricaine and benzocaine were 26.1% and 39.1%, respectively, with detected mass fraction ranges of 2.07-6.34 μg·kg^-1 and 1.44-2.87 μg·kg^-1, respectively. This method has good practicability and can provide reference for the high-throughput residue analysis of the 16 kinds of anesthetics in fish muscle.

Key words: magnetic nano material, liquid chromatography-tandem mass spectrometry(LC-MS/MS), anesthetic, fish

中图分类号:

TS254.7

王美玉, 刘真真, 王新全, 王娇, 刘小琦, 谷晨舒, 杜丽慧, 齐沛沛. 磁分散固相萃取结合LC⁃MS/MS分析鱼肌肉中16种麻醉剂残留量[J]. 浙江农业学报, 2026, 38(1): 148-159.

WANG Meiyu, LIU Zhenzhen, WANG Xinquan, WANG Jiao, LIU Xiaoqi, GU Chenshu, DU Lihui, QI Peipei. Determination of 16 anesthetic residues in fish muscle by magnetic dispersive solid-phase extraction combined with LC-MS/MS[J]. Acta Agriculturae Zhejiangensis, 2026, 38(1): 148-159.

图/表 11

参考文献 31

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化合物 Compound	CAS号 CAS number	化学式 Chemical formula	保留时间/min Retention time/min	母离子(m/z) Parent ions(m/z)	子离子(m/z) Product ions(m/z)	碰撞能量/eV Collision energy/eV
三卡因MS-222	886-86-2	C₁₀H₁₅NO₅S	3.73	166.2	138.3^*, 120.0	-22,-24
丁卡因Tetracaine	94-24-6	C₁₅H₂₄N₂O₂	3.67	265.2	176.2^*, 72.1	-21,-40
普鲁卡因Procaine	59-46-1	C₁₃H₂₀N₂O₂	2.42	237.2	100.2^*, 164.4	-22,-23
利多卡因Lidocaine	137-58-6	C₁₄H₂₂N₂O	3.06	235.1	85.9^*, 99.0	-27,-31
苯佐卡因Benzocaine	94-09-7	C₉H₁₁NO₂	3.75	166.1	138.1^*, 94.0	-18,-24
布比卡因Bupivacaine	2180-92-9	C₁₈H₂₈N₂O	3.63	289.2	140.2^*,98.0	-24,-54
奥沙西泮Oxazepam	604-75-1	C₁₅H₁₁ClN₂O₂	4.12	287.2	241.1^*,193.1	-30,-21
地西泮Diazepam	439-14-5	C₁₆H₁₃ClN₂O	4.33	285.1	193.1^*,154.1	-32,-28
去甲地西泮Nordiazepam	1088-11-5	C₁₅H₁₁ClN₂O	4.26	271.0	140.0^*,165.0	-20,-20
替马西泮Temazepam	846-50-4	C₁₆H₁₃ClN₂O₂	4.18	301.0	254.9^*,177.0	-13,-34
硝西泮Nitrazepam	146-22-5	C₁₅H₁₁N₃O₃	4.02	282.1	236.0^*,180.0	-34,-52
阿普唑仑Alprazolam	28981-97-7	C₁₇H₁₃ClN₄	4.13	309.1	281.1^*,205.0	-39,-55
三唑仑Triazolam	28911-01-5	C₁₇H₁₂Cl₂N₄	4.08	343.1	308.1^*,239.0	-36,-55
异丙嗪Promethazine	60-87-7	C₁₇H₂₀N₂S	3.86	285.2	86.1^*,198.1	-25,-31
丙酰丙嗪Propionylpromazine	7681-67-6	C₂₀H₂₅ClN₂OS	3.99	341.2	100.2^*,164.4	-22,-23
异丙嗪亚砜Promethazine sulfoxide	7640-51-9	C₁₇H₂₀N₂OS	3.21	301.2	86.1^*,198.1	-32,-34

化合物 Compound	CAS号 CAS number	化学式 Chemical formula	保留时间/min Retention time/min	母离子(m/z) Parent ions(m/z)	子离子(m/z) Product ions(m/z)	碰撞能量/eV Collision energy/eV
三卡因MS-222	886-86-2	C₁₀H₁₅NO₅S	3.73	166.2	138.3^*, 120.0	-22,-24
丁卡因Tetracaine	94-24-6	C₁₅H₂₄N₂O₂	3.67	265.2	176.2^*, 72.1	-21,-40
普鲁卡因Procaine	59-46-1	C₁₃H₂₀N₂O₂	2.42	237.2	100.2^*, 164.4	-22,-23
利多卡因Lidocaine	137-58-6	C₁₄H₂₂N₂O	3.06	235.1	85.9^*, 99.0	-27,-31
苯佐卡因Benzocaine	94-09-7	C₉H₁₁NO₂	3.75	166.1	138.1^*, 94.0	-18,-24
布比卡因Bupivacaine	2180-92-9	C₁₈H₂₈N₂O	3.63	289.2	140.2^*,98.0	-24,-54
奥沙西泮Oxazepam	604-75-1	C₁₅H₁₁ClN₂O₂	4.12	287.2	241.1^*,193.1	-30,-21
地西泮Diazepam	439-14-5	C₁₆H₁₃ClN₂O	4.33	285.1	193.1^*,154.1	-32,-28
去甲地西泮Nordiazepam	1088-11-5	C₁₅H₁₁ClN₂O	4.26	271.0	140.0^*,165.0	-20,-20
替马西泮Temazepam	846-50-4	C₁₆H₁₃ClN₂O₂	4.18	301.0	254.9^*,177.0	-13,-34
硝西泮Nitrazepam	146-22-5	C₁₅H₁₁N₃O₃	4.02	282.1	236.0^*,180.0	-34,-52
阿普唑仑Alprazolam	28981-97-7	C₁₇H₁₃ClN₄	4.13	309.1	281.1^*,205.0	-39,-55
三唑仑Triazolam	28911-01-5	C₁₇H₁₂Cl₂N₄	4.08	343.1	308.1^*,239.0	-36,-55
异丙嗪Promethazine	60-87-7	C₁₇H₂₀N₂S	3.86	285.2	86.1^*,198.1	-25,-31
丙酰丙嗪Propionylpromazine	7681-67-6	C₂₀H₂₅ClN₂OS	3.99	341.2	100.2^*,164.4	-22,-23
异丙嗪亚砜Promethazine sulfoxide	7640-51-9	C₁₇H₂₀N₂OS	3.21	301.2	86.1^*,198.1	-32,-34

化合物 Compound	线性方程 Linear regression equation	线性范围/(μg·kg^-1) Linear range/ (μg·kg^-1)	相关系数 Correlation coefficient	基质效应 Matrix effect	检出限/(μg·kg^-1) Limit of detection/ (μg·kg^-1)
三卡因MS-222	Y=19 878X+19 312	0.5~200.0	0.999	0.83	0.57
	Y=24 069X+50 404	0.5~200.0	0.999		0.54
丁卡因Tetracaine	Y=311 769X+105 029	0.5~200.0	0.998	0.97	0.48
	Y=322 563X+7 290.8	0.5~200.0	0.999		0.52
普鲁卡因Procaine	Y=45 380X-21 710	0.5~200.0	0.998	1.06	0.44
	Y=42 921X-10 776	0.5~200.0	0.996		0.40
利多卡因Lidocaine	Y=274 357X-41 908	5.0~200.0	0.997	1.02	0.23
	Y=267 923X-53 578	5.0~200.0	0.998		0.25
苯佐卡因Benzocaine	Y=8 613.5X+741.44	0.5~200.0	1.000	0.85	0.42
	Y=10 130X+18 205	0.5~200.0	0.999		0.23
布比卡因Bupivacaine	Y=58 886X+148 900	2.0~200.0	0.997	1.05	0.08
	Y=56 115X-96 312	2.0~200.0	0.998		0.26
奥沙西泮Oxazepam	Y =1 772.9X-4 791.9	5.0~200.0	0.996	0.87	0.48
	Y=2 031.8X-5 816.1	5.0~200.0	0.997		0.44
地西泮Diazepam	Y=6 992.7X +2 291.2	1.0~200.0	0.996	0.88	0.50
	Y=7 948.1X-4 991.2	1.0~200.0	0.999		0.52
去甲地西泮Nordiazepam	Y=696.52X-1 346.3	2.0~200.0	0.999	0.93	0.33
	Y=752.32X+48.125	2.0~200.0	0.999		0.47
替马西泮Temazepam	Y=1 731.6 X-353.52	0.5~200.0	0.999	0.97	0.26
	Y=1 793.8X-320.5	0.5~200.0	0.996		0.41
硝西泮Nitrazepam	Y=975.71X+1 105.3	2.0~200.0	0.997	0.95	0.52
	Y=1 029.8X-2 018.5	2.0~200.0	0.998		0.39
阿普唑仑Alprazolam	Y=3 452X-855.7	0.5~200.0	0.999	0.92	0.46
	Y=3 745.5X-691.1	0.5~200.0	0.997		0.47
三唑仑Triazolam	Y=3 952.3X-158.53	0.5~200.0	0.999	1.05	0.32
	Y=3 747.9X+554.04	0.5~200.0	0.999		0.29
异丙嗪Promethazine	Y=23 559X-41 867	2.0~200.0	0.999	1.02	0.28
	Y=23 207X-21 523	2.0~200.0	0.999		0.23
丙酰丙嗪Propionylpromazine	Y=19 165X-22 787	2.0~200.0	0.998	1.03	0.33
	Y=18 539X-20 557	2.0~200.0	0.999		0.17
异丙嗪亚砜	Y=5 951.2X-5 675.2	2.0~200.0	1.000	1.01	0.38
Promethazine sulfoxide	Y=5 892.5X-8 374.2	2.0~200.0	0.999		0.29

化合物 Compound	线性方程 Linear regression equation	线性范围/(μg·kg^-1) Linear range/ (μg·kg^-1)	相关系数 Correlation coefficient	基质效应 Matrix effect	检出限/(μg·kg^-1) Limit of detection/ (μg·kg^-1)
三卡因MS-222	Y=19 878X+19 312	0.5~200.0	0.999	0.83	0.57
	Y=24 069X+50 404	0.5~200.0	0.999		0.54
丁卡因Tetracaine	Y=311 769X+105 029	0.5~200.0	0.998	0.97	0.48
	Y=322 563X+7 290.8	0.5~200.0	0.999		0.52
普鲁卡因Procaine	Y=45 380X-21 710	0.5~200.0	0.998	1.06	0.44
	Y=42 921X-10 776	0.5~200.0	0.996		0.40
利多卡因Lidocaine	Y=274 357X-41 908	5.0~200.0	0.997	1.02	0.23
	Y=267 923X-53 578	5.0~200.0	0.998		0.25
苯佐卡因Benzocaine	Y=8 613.5X+741.44	0.5~200.0	1.000	0.85	0.42
	Y=10 130X+18 205	0.5~200.0	0.999		0.23
布比卡因Bupivacaine	Y=58 886X+148 900	2.0~200.0	0.997	1.05	0.08
	Y=56 115X-96 312	2.0~200.0	0.998		0.26
奥沙西泮Oxazepam	Y =1 772.9X-4 791.9	5.0~200.0	0.996	0.87	0.48
	Y=2 031.8X-5 816.1	5.0~200.0	0.997		0.44
地西泮Diazepam	Y=6 992.7X +2 291.2	1.0~200.0	0.996	0.88	0.50
	Y=7 948.1X-4 991.2	1.0~200.0	0.999		0.52
去甲地西泮Nordiazepam	Y=696.52X-1 346.3	2.0~200.0	0.999	0.93	0.33
	Y=752.32X+48.125	2.0~200.0	0.999		0.47
替马西泮Temazepam	Y=1 731.6 X-353.52	0.5~200.0	0.999	0.97	0.26
	Y=1 793.8X-320.5	0.5~200.0	0.996		0.41
硝西泮Nitrazepam	Y=975.71X+1 105.3	2.0~200.0	0.997	0.95	0.52
	Y=1 029.8X-2 018.5	2.0~200.0	0.998		0.39
阿普唑仑Alprazolam	Y=3 452X-855.7	0.5~200.0	0.999	0.92	0.46
	Y=3 745.5X-691.1	0.5~200.0	0.997		0.47
三唑仑Triazolam	Y=3 952.3X-158.53	0.5~200.0	0.999	1.05	0.32
	Y=3 747.9X+554.04	0.5~200.0	0.999		0.29
异丙嗪Promethazine	Y=23 559X-41 867	2.0~200.0	0.999	1.02	0.28
	Y=23 207X-21 523	2.0~200.0	0.999		0.23
丙酰丙嗪Propionylpromazine	Y=19 165X-22 787	2.0~200.0	0.998	1.03	0.33
	Y=18 539X-20 557	2.0~200.0	0.999		0.17
异丙嗪亚砜	Y=5 951.2X-5 675.2	2.0~200.0	1.000	1.01	0.38
Promethazine sulfoxide	Y=5 892.5X-8 374.2	2.0~200.0	0.999		0.29

化合物 Compound	日内回收率(相对标准偏差) Intra-day recovery rate (RSD)			日间回收率(相对标准偏差) Inter-day recovery rate(RSD)
化合物 Compound	1 μg·kg^-1	10 μg·kg^-1	100 μg·kg^-1	1 μg·kg^-1	10 μg·kg^-1	100 μg·kg^-1
三卡因Tricaine	84.4(6.9)	88.6(2.0)	99.2(5.6)	84.7(4.0)	91.1(3.3)	83.5(2.3)
丁卡因Tetracaine	79.3(1.1)	95.9(4.1)	98.5(6.4)	95.9(1.1)	83.6(4.1)	91.3(6.2)
普鲁卡因Procaine	82.1(2.8)	82.9(0.4)	81.2(6.7)	87.7(6.4)	89.2(2.4)	81.2(6.7)
利多卡因Lidocaine	96.4(6.3)	91.0(3.3)	99.4(3.6)	97.2(3.3)	99.8(1.4)	100.2(3.5)
苯佐卡因Benzocaine	81.3(2.0)	77.4(3.8)	97.4(3.9)	103.8(2.0)	87.8(3.8)	92.8(1.1)
布比卡因Bupivacaine	76.9(5.7)	74.4(6.1)	76.9(3.9)	81.4(1.5)	98.0(1.8)	110.8(4.7)
奥沙西泮Oxazepam	82.9(0.8)	87.6(7.2)	97.3(3.4)	78.9(8.1)	89.3(3.3)	101.8(6.5)
地西泮Diazepam	74.9(4.9)	110.8(2.6)	108.4(3.8)	87.3(3.9)	84.3(8.4)	77.9(8.1)
去甲地西泮Nordiazepam	85.6(4.1)	92.4(0.6)	99.8(6.7)	75.4(3.7)	97.8(7.4)	89.9(8.3)
替马西泮Temazepam	79.8(3.7)	108.3(4.8)	88.1(6.7)	85.9(7.6)	76.9(8.1)	107.5(4.4)
硝西泮Nitrazepam	72.4(3.4)	79.2(7.7)	89.9(5.1)	75.1(3.9)	97.7(5.5)	110.3(1.4)
阿普唑仑Alprazolam	79.1(3.6)	84.1(5.3)	109.2(4.7)	87.4(6.3)	98.0(4.0)	96.7(2.9)
三唑仑Triazolam	77.2(7.3)	85.3(6.8)	99.9(5.3)	90.3(6.1)	81.4(2.4)	86.4(3.6)
异丙嗪Promethazine	76.9(4.0)	101.3(5.9)	87.3(2.0)	91.9(6.6)	92.8(4.6)	103.3(3.1)
丙酰丙嗪Propionylpromazine	75.7(3.9)	90.9(7.5)	76.4(3.7)	89.7(5.8)	92.0(6.0)	106.4(4.9)
异丙嗪亚砜Promethazine sulfoxide	85.3(0.8)	100.2(4.4)	87.5(3.8)	74.0(6.9)	81.3(2.8)	96.8(5.7)

磁分散固相萃取结合LC⁃MS/MS分析鱼肌肉中16种麻醉剂残留量

Determination of 16 anesthetic residues in fish muscle by magnetic dispersive solid-phase extraction combined with LC-MS/MS

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参考文献 31

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预处理方法 Preparation method	吸附剂数量 Adsorbent amounts	单个样品处理时间/min Single pretreatment time/min	检出限/(μg·kg^-1) Limit of detection/ (μg·kg^-1)	基质效应 Matrix effect	回收率/% Recovery rate/%	参考文献 Reference
SPE	Oasis PRiME HLB(150 mg/3 mL)	22	1.50~6.00	0.58~0.85	76.8~110.0	[30]
DSPE	50 mg PSA+10 mg C₁₈+20 mg PS-GMA	24	11.00~43.00	0.87~1.23	79.7~109.0	[31]
MDSPE	20 mg Fe₃O₄-PLS+10 mg PSA	7.5	0.08~0.57	0.83~1.06	72.4~110.8	本文This study

序号 No.	样品 Sample	三卡因 MS-222	苯佐卡因 Benzocaine
1	鳙鱼Hypophthalmichthys nobilis	ND	ND
2	鳙鱼Hypophthalmichthys nobilis	ND	ND
3	白条鱼Chanodichthys erythropterus	ND	1.44
4	鳙鱼Hypophthalmichthys nobilis	ND	ND
5	鳊鱼Megalobrama amblycephala	ND	ND
6	花链Hypophthalmichthys nobilis	ND	ND
7	鲫鱼Carassius auratus	ND	ND
8	黑鱼Channa argus	ND	ND
9	草鱼Ctenopharyngodon idella	ND	1.47
10	光唇鱼Acrossocheilus fasciatus	ND	1.50
11	光唇鱼Acrossocheilus fasciatus	ND	ND
12	光唇鱼Acrossocheilus fasciatus	ND	ND
13	光唇鱼Acrossocheilus fasciatus	ND	ND
14	马口鱼Opsariichthys bidens	ND	ND
15	马口鱼Opsariichthys bidens	ND	ND
16	光唇鱼Acrossocheilus fasciatus	2.07	ND
17	光唇鱼Acrossocheilus fasciatus	2.15	1.53
18	鲫鱼Carassius auratus	2.31	1.61
19	马口鱼Opsariichthys bidens	ND	1.72
20	马口鱼Opsariichthys bidens	ND	1.78
21	胖头鱼Hypophthalmichthys nobilis	3.98	1.80
22	胖头鱼Hypophthalmichthys nobilis	5.76	2.87
23	鲫鱼Carassius auratus	6.34	ND

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