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

doi:10.3969/j.issn.1004-1524.20250048

Acta Agriculturae Zhejiangensis ›› 2026, Vol. 38 ›› Issue (1): 148-159.DOI: 10.3969/j.issn.1004-1524.20250048

• Quality and Safety of Agricultural Products • Previous Articles Next Articles

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

Abstract

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

CLC Number:

TS254.7

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.

Figures/Tables 11

References 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)

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

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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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