Determination of Aldicarb， Aldicarb Sulfoxide， Aldicarb Sulfone in Water by Solid Phase Extraction and UPLC⁃MS/MS with Isotope Dilution

doi:10.19894/j.issn.1000-0518.210279

Chinese Journal of Applied Chemistry ›› 2022, Vol. 39 ›› Issue (3): 470-479.DOI: 10.19894/j.issn.1000-0518.210279

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Determination of Aldicarb， Aldicarb Sulfoxide， Aldicarb Sulfone in Water by Solid Phase Extraction and UPLC⁃MS/MS with Isotope Dilution

Hui-Jing SUN(), Dong-Ni CUI

State Environmental Protection Key Laboratory of Monitoring and Analysis for Organic Pollutants in Surface Water，Jiangsu Provincial Environmental Monitoring Center，Nanjing 210019，China

Received:2021-06-09 Accepted:2021-09-02 Published:2022-03-01 Online:2022-03-15
Contact: Hui-Jing SUN
About author:516482697@qq.com
Supported by:
Jiangsu Environmental Monitoring Research Fund Project 2019 （No.1909）

Abstract

Abstract:

A method for analysis of aldicarb， aldicarb sulfoxide and aldicarb sulfone in water was developed using solid phase extraction and HPLC-MS/MS with isotope dilution. The aqueous samples were spiked with isotope-labeled internal standards aldicarb-D₃， aldicarb sulfoxide-D₃ and aldicarb sulfone-D₃， concentrated and purified on an HLB cartridge， and then separated on a Waters ACQUITY UPLC^TM BEH C₁₈ column by gradient elution with 0.1% formic acid-5 mmol/L ammonium acetate-acetonitrile as the mobile phase. The analytes were detected by positive electrospray ionization with multiple reaction monitoring （MRM）. The internal standard method was used to determine the results. There is a good linearity for target compounds in the range of 0.5~200 μg/L with the correlation coefficient （r） larger than 0.999. The method detection limit （MDL） is 0.0008~0.001 μg/L. The average recoveries range between 94.5%~105% at three different spiked levels. The relative standard deviation （RSD） is between 2.7%~6.5%. The method is sensitive and accurate， and is suitable for determination of aldicarb， aldicarb sulfoxide， aldicarb sulfone in water.

Key words: Aldicarb, Aldicarb sulfoxide, Aldicarb sulfone, Solid phase extration, Conversion, High performance liquid chromatography-mass spectrometry

CLC Number:

O661.1

Hui-Jing SUN, Dong-Ni CUI. Determination of Aldicarb， Aldicarb Sulfoxide， Aldicarb Sulfone in Water by Solid Phase Extraction and UPLC⁃MS/MS with Isotope Dilution[J]. Chinese Journal of Applied Chemistry, 2022, 39(3): 470-479.

Figures/Tables 16

References 20

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化合物 Compound	母离子 Parent ion （m/z）	子离子 Daughter ion （m/z）	去簇电压 Declustering potential/V	碰撞能量 Collison energy/eV
涕灭威 Aldicarb	208.0	116.0	20	11
涕灭威砜 Aldicarb sulfone	240.0	148.1	25	17
涕灭威亚砜 Aldicarb sulfoxide	224.0	132.0	30	14
涕灭威?D₃ Aldicarb?D₃	211.1	89.2	40	24
涕灭威砜?D₃ Aldicarb sulfone?D₃	226.0	86.2	40	22
涕灭威亚砜?D₃ Aldicarb sulfoxide?D₃	210.0	132	20	9

化合物 Compound	母离子 Parent ion （m/z）	子离子 Daughter ion （m/z）	去簇电压 Declustering potential/V	碰撞能量 Collison energy/eV
涕灭威 Aldicarb	208.0	116.0	20	11
涕灭威砜 Aldicarb sulfone	240.0	148.1	25	17
涕灭威亚砜 Aldicarb sulfoxide	224.0	132.0	30	14
涕灭威?D₃ Aldicarb?D₃	211.1	89.2	40	24
涕灭威砜?D₃ Aldicarb sulfone?D₃	226.0	86.2	40	22
涕灭威亚砜?D₃ Aldicarb sulfoxide?D₃	210.0	132	20	9

化合物 Compound	回收率 Recovery/%
化合物 Compound	C18	HLB
涕灭威 Aldicarb	56.4	95.6
涕灭威亚砜 Aldicarb sulfoxide	49.8	108
涕灭威砜 Aldicarb sulfone	52.5	98.4

化合物 Compound	回收率 Recovery/%
化合物 Compound	C18	HLB
涕灭威 Aldicarb	56.4	95.6
涕灭威亚砜 Aldicarb sulfoxide	49.8	108
涕灭威砜 Aldicarb sulfone	52.5	98.4

化合物 Compound	回收率 Recovery/%
化合物 Compound	pH=4	pH=7
涕灭威 Aldicarb	94.3	95.6
涕灭威亚砜 Aldicarb sulfoxide	110	108
涕灭威砜 Aldicarb sulfone	96.0	98.4

Determination of Aldicarb， Aldicarb Sulfoxide， Aldicarb Sulfone in Water by Solid Phase Extraction and UPLC⁃MS/MS with Isotope Dilution

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Figures/Tables 16

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洗脱体积/mL Elution volume/mL	回收率 Recovery/%
洗脱体积/mL Elution volume/mL	涕灭威 Aldicarb	涕灭威亚砜 Aldicarb sulfoxide	涕灭威砜 Aldicarb sulfone
3.0	96.1	106	98.5
4.0	95.6	108	98.4
6.0	93.9	107	97.9
9.9	96.2	110	96.8

上样速度 Loading speed/（mL·min^-1）	涕灭威 Aldicarb		涕灭威亚砜 Aldicarb sulfoxide		涕灭威砜 Aldicarb sulfone
上样速度 Loading speed/（mL·min^-1）	回收率 Recovery/%	相对标准偏差 RSD/%	回收率 Recovery/%	相对标准偏差 RSD/%	回收率 Recovery/%	相对标准偏差 RSD/%
5	96.0	3.2	112	2.9	98.2	3.7
10	95.6	2.9	108	3.1	98.4	3.6
15	95.1	8.3	95.3	13.2	103	11.2

化合物 Analyte	0.02 μg/L		0.20 μg/L		1.00 μg/L
化合物 Analyte	平均回收率 Recovery/%	相对标准偏差 RSD/%	平均回收率 Recovery/%	相对标准偏差 RSD/%	平均回收率 Recovery/%	相对标准偏差 RSD/%
涕灭威 Aldicarb	94.5	5.4	96.6	3.7	97.4	4.9
涕灭威亚砜Aldicarb sulfoxide	98.1	6.5	105	5.8	108	3.6
涕灭威砜 Aldicarb sulfone	99.0	5.9	97.8	4.7	98.2	5.4

化合物 Compound	样品含量 Sample content/（μg·L^-1）	加标量 Added/（μg·L^-1）	测得量 Measured quantity/（μg·L^-1）	回收率 Recovery/%
涕灭威 Aldicarb	ND	0.050	0.047	94.8
	ND	0.050	0.049	97.8
	ND	0.050	0.049	97.4
涕灭威砜 Aldicarb sulfone	ND	0.050	0.045	90.4
	ND	0.050	0.046	92.0
	ND	0.050	0.046	92.2
涕灭威亚砜 Aldicarb sulfoxide	ND	0.050	0.058	115
	ND	0.050	0.058	117
	ND	0.050	0.058	116

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