通过式固相萃取净化-超高效液相色谱-串联质谱法测定液体乳中10种氨基甲酸酯类农药残留

doi:10.3724/SP.J.1123.2023.03017

色谱 ›› 2023, Vol. 41 ›› Issue (9): 807-813.DOI: 10.3724/SP.J.1123.2023.03017

通过式固相萃取净化-超高效液相色谱-串联质谱法测定液体乳中10种氨基甲酸酯类农药残留

岳超¹, 赵超群¹, 毛思浩¹, 王展华¹, 施贝¹, 徐欣丰², 梁晶晶¹^,^*()

1.浙江省食品药品检验研究院, 国家市场监管重点实验室(功能食品质量与安全领域), 浙江省市场局重点实验室(保健食品质量安全重点实验室), 浙江杭州 310052
2.浙江中医药大学, 浙江杭州 310056

收稿日期:2023-03-28 出版日期:2023-09-08 发布日期:2023-09-15
通讯作者: *Tel:(0571)87180325,E-mail:liangjingjing@zjyj.org.cn.
基金资助:
浙江省科技厅分析测试项目(LGC22H280007);浙江省市场监督管理局“雏鹰计划”项目(ZC2021A028);浙江省药品监督管理局项目(2023020)

Determination of 10 carbamate pesticide residues in liquid milk by ultra performance liquid chromatography-tandem mass spectrometry with pass-through solid-phase extraction purification

YUE Chao¹, ZHAO Chaoqun¹, MAO Sihao¹, WANG Zhanhua¹, SHI Bei¹, XU Xinfeng², LIANG Jingjing¹^,^*()

1. Zhejiang Institute of Food and Drug Control, Key Laboratory of Functional Food Nutrition and Quality Safety for State Market Regulation, Key Laboratory of Health Food Quality Safety of Provincial Market Regulation, Hangzhou 310052, China
2. Zhejiang Chinese Medical University, Hangzhou 310056, China

Received:2023-03-28 Online:2023-09-08 Published:2023-09-15
Supported by:
Analysis and Testing Subject Fund of Zhejiang Provincial Department of Science and Technology(LGC22H280007);“Eagle Project” Fund of Zhejiang Provincial Market Supervision Administration(ZC2021A028);Subject Fund of Zhejiang Medical Products Administration(2023020)

摘要/Abstract

摘要：

建立了应用直接通过式的增强型基质脂质去除柱联合超高效液相色谱-串联质谱法快速测定乳品中10种氨基甲酸酯类农药残留的分析方法。样品采用乙腈为提取液,沉淀除去蛋白质后,上清液通过Captiva EMR-Lipid柱净化,使用ACQUITY UPLC BEH C₁₈柱(100 mm×2.1 mm, 1.7 μm)进行分离,以甲醇-0.1%甲酸水溶液为流动相进行梯度洗脱,流速0.3 mL/min,柱温35 ℃,采用电喷雾正离子模式(ESI⁺)和多反应监测(MRM)扫描方式检测,基质标准曲线外标法定量分析。结果显示,10种氨基甲酸酯类农药在2~200 μg/L范围内线性关系良好,相关系数(r)>0.999,方法的检出限为0.045~0.23 μg/kg,定量限为0.15~0.77 μg/kg;在空白基质中添加3个水平(15、50、100 μg/kg)的10种氨基甲酸酯类农药,进行加标回收率和重复性试验,回收率为68.7%~93.3%,相对标准偏差(RSD)为1.8%~8.0%。由结果可知,本研究方法高效、便捷、准确,适用于乳品中10种氨基甲酸酯类农药的批量检测。将本研究结果与现行国标测定方法中的氨基柱和ENVI^TM-18 SPE柱净化效果进行比较,结果表明,经过Captiva EMR-Lipid直接通过式柱净化后,涕灭威及其代谢产物和甲萘威的回收率提升均在20%以上,本研究方法更适用于相对极性较强的氨基甲酸酯类农药,测定结果的重复性好,准确率高。

关键词: 增强型基质脂质去除, 通过式固相萃取净化, 超高效液相色谱-串联质谱, 氨基甲酸酯类农药, 液体乳

Abstract:

Carbamates are used in broad-spectrum insecticides and herbicides, and have highly efficient, low-residue, and long-lasting characteristics. However, this type of pesticide exerts mutagenic, teratogenic, carcinogenic, and other adverse effects, and its frequent use can exceed the recommended scope and limits. Research on the determination of carbamate pesticides mainly focuses on foods of plant origin and pays less attention to foods of animal origin. The methods for carbamate determination described in the current national standards have complicated operating procedures and low efficiency. Therefore, highly efficient and accurate methods for carbamate detection in milk must be established. In this work, a rapid method based on pass-through solid-phase extraction (SPE) purification coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of 10 carbamate pesticides in liquid milk. The pretreatment and instrument methods were systematically optimized. The milk sample was extracted with acetonitrile, and then purified using a Captiva EMR-Lipid filtration kit. The purified extract was separated on an ACQUITY UPLC BEH C₁₈ column with mobile phase of methanol and 0.1% formic acid aqueous solution in gradient elution. The flow rate was 0.3 mL/min. Column temperature was 35 ℃. Quantitative analysis was performed using the external standard method with matrix matching curves. The 10 carbamate pesticides showed good linear relationships in the mass concentration range of 2-200 μg/L, with correlation coefficients greater than 0.999. The limits of detection (LODs) and quantification (LOQs) for the 10 carbamate pesticides were 0.045-0.23 and 0.15-0.77 μg/kg, respectively. Recovery tests were conducted using the blank-matrix method at three spiked levels of 15, 50, and 100 μg/kg, and good recoveries for the 10 carbamate pesticides were obtained. In particular, the recoveries for the three spiked levels of 15, 50, and 100 μg/kg were 68.7%-93.3% with relative standard deviations (RSDs) of 1.8%-8.0%. The proposed method is efficient, convenient, accurate, and suitable for the rapid detection of the 10 carbamate pesticides in liquid milk. Compared with the conventional NH₂ and ENVI^TM-18 SPE columns used in the national standard determination method, the proposed method demonstrated better purification effects. The recoveries for aldicarb sulfoxide, aldicarb sulfone, methomyl, and carbaryl after purification using the Captiva EMR-Lipid kit increased from 60% to 80%. Thus, the proposed method is suitable for targets with strong polarity and gives measurement results with good repeatability and accuracy.

Key words: enhanced matrix removal-lipid cleaning, pass-through solid-phase extraction purification, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), carbamate pesticide, liquid milk

中图分类号:

O658

岳超, 赵超群, 毛思浩, 王展华, 施贝, 徐欣丰, 梁晶晶. 通过式固相萃取净化-超高效液相色谱-串联质谱法测定液体乳中10种氨基甲酸酯类农药残留[J]. 色谱, 2023, 41(9): 807-813.

YUE Chao, ZHAO Chaoqun, MAO Sihao, WANG Zhanhua, SHI Bei, XU Xinfeng, LIANG Jingjing. Determination of 10 carbamate pesticide residues in liquid milk by ultra performance liquid chromatography-tandem mass spectrometry with pass-through solid-phase extraction purification[J]. Chinese Journal of Chromatography, 2023, 41(9): 807-813.

图/表 5

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Compound	t_R/ min	Precursor ion (m/z)	Daughter ion (m/z)	DP/ V	CE/ V
Aldicarb sulfoxide	4.03	207.1	132.0^*	55	9
			89.2		20
Aldicarb sulfone	4.47	210.1	118.0^*	30	17
			166.1		16
Methomyl	4.64	163.1	88.0^*	38	12
			106.3		14
3-Hydroxy carbofuran	5.41	238.1	181.1^*	70	16
			163.1		18
Aldicarb	6.15	208.1	116.1^*	20	11
			89.3		25
Metolcarb	6.41	166.1	109.3^*	80	16
			20.4		23
Carbofuran	6.74	222.1	165.1^*	70	16
			123.3		29
Carbaryl	6.91	202.1	145.3^*	100	17
			127.1		42
Isoprocarb	7.27	194.1	137.5^*	110	12
			94.5		21
Fenobucarb	7.86	207.9	94.7^*	90	23
			151.5		43

Compound	t_R/ min	Precursor ion (m/z)	Daughter ion (m/z)	DP/ V	CE/ V
Aldicarb sulfoxide	4.03	207.1	132.0^*	55	9
			89.2		20
Aldicarb sulfone	4.47	210.1	118.0^*	30	17
			166.1		16
Methomyl	4.64	163.1	88.0^*	38	12
			106.3		14
3-Hydroxy carbofuran	5.41	238.1	181.1^*	70	16
			163.1		18
Aldicarb	6.15	208.1	116.1^*	20	11
			89.3		25
Metolcarb	6.41	166.1	109.3^*	80	16
			20.4		23
Carbofuran	6.74	222.1	165.1^*	70	16
			123.3		29
Carbaryl	6.91	202.1	145.3^*	100	17
			127.1		42
Isoprocarb	7.27	194.1	137.5^*	110	12
			94.5		21
Fenobucarb	7.86	207.9	94.7^*	90	23
			151.5		43

Compound	Linear range/(μg/L)	Linear equation	r	LOD/(μg/kg)	LOQ/(μg/kg)
Aldicarb sulfoxide	2-200	y=6.92×10x+2.35×10⁴	1.0000	0.045	0.15
Aldicarb sulfone	2-200	y=1.08×10⁴x-1.40×10⁴	0.9996	0.046	0.15
Methomyl	2-200	y=3.50×10⁴x-5.99×10⁴	0.9996	0.23	0.76
3-Hydroxy carbofuran	2-200	y=7.20×10⁴x+9.10×10⁴	0.9997	0.23	0.76
Aldicarb	2-200	y=1.48×10⁵x-4.40×10⁵	0.9993	0.045	0.15
Metolcarb	2-200	y=9.98×10⁴x+6.70×10⁴	1.0000	0.22	0.76
Carbofuran	2-200	y=7.33×10⁴x+3.96×10⁵	0.9999	0.23	0.76
Carbaryl	2-200	y=4.34×10⁴x+1.90×10⁴	0.9999	0.21	0.76
Isoprocarb	2-200	y=2.07×10⁵x-3.39×10⁵	1.0000	0.22	0.77
Fenobucarb	2-200	y=4.15×10⁵x+1.09×10⁵	0.9999	0.23	0.76

Compound	Linear range/(μg/L)	Linear equation	r	LOD/(μg/kg)	LOQ/(μg/kg)
Aldicarb sulfoxide	2-200	y=6.92×10x+2.35×10⁴	1.0000	0.045	0.15
Aldicarb sulfone	2-200	y=1.08×10⁴x-1.40×10⁴	0.9996	0.046	0.15
Methomyl	2-200	y=3.50×10⁴x-5.99×10⁴	0.9996	0.23	0.76
3-Hydroxy carbofuran	2-200	y=7.20×10⁴x+9.10×10⁴	0.9997	0.23	0.76
Aldicarb	2-200	y=1.48×10⁵x-4.40×10⁵	0.9993	0.045	0.15
Metolcarb	2-200	y=9.98×10⁴x+6.70×10⁴	1.0000	0.22	0.76
Carbofuran	2-200	y=7.33×10⁴x+3.96×10⁵	0.9999	0.23	0.76
Carbaryl	2-200	y=4.34×10⁴x+1.90×10⁴	0.9999	0.21	0.76
Isoprocarb	2-200	y=2.07×10⁵x-3.39×10⁵	1.0000	0.22	0.77
Fenobucarb	2-200	y=4.15×10⁵x+1.09×10⁵	0.9999	0.23	0.76

Compound	Added/ (μg/kg)	Found/ (μg/kg)	Recovery/ %	RSD/ %	Compound	Added/ (μg/kg)	Found/ (μg/kg)	Recovery/ %	RSD/ %
Aldicarb sulfoxide	15	13.3	88.7	6.5	Metolcarb	15	13.5	90.0	4.5
	50	42.1	84.2	5.9		50	38.4	76.7	5.1
	100	79.3	79.3	6.7		100	77.6	77.6	4.9
Aldicarb sulfone	15	13.0	86.7	3.9	Carbofuran	15	12.7	84.7	6.0
	50	45.1	90.2	4.8		50	46.4	92.7	5.1
	100	92.7	92.7	6.8		100	89.9	89.9	2.5
Methomyl	15	11.5	76.7	5.3	Carbaryl	15	10.9	72.7	4.8
	50	38.4	76.8	2.7		50	35.3	70.5	4.1
	100	74.2	74.2	4.6		100	68.7	68.7	8.0
3-Hydroxy carbofuran	15	12.1	80.7	4.0	Isoprocarb	15	13.0	86.7	3.9
	50	43.0	85.9	1.8		50	40.8	81.5	5.8
	100	83.1	83.1	2.6		100	84.6	84.6	4.8
Aldicarb	15	11.6	77.3	4.6	Fenobucarb	15	14.0	93.3	4.8
	50	38.1	76.2	4.6		50	43.3	86.5	3.5
	100	70.8	70.8	5.7		100	82.6	82.6	5.5

通过式固相萃取净化-超高效液相色谱-串联质谱法测定液体乳中10种氨基甲酸酯类农药残留

Determination of 10 carbamate pesticide residues in liquid milk by ultra performance liquid chromatography-tandem mass spectrometry with pass-through solid-phase extraction purification

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