Determination of carbendazim residues in Procambarus clarkii by high performance liquid chromatography-triple quadrupole mass spectrometry

doi:10.3724/SP.J.1123.2019.10009

Abstract

Abstract:

A novel method based on high performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS) was established for the determination of carbendazim in Procambarus clarkii. The sample was extracted by ethyl acetate under alkaline conditions and centrifuged. The supernatant was concentrated by rotary evaporation, redissolved, and then enriched and purified on a mixed-mode cation exchange solid phase extraction column (MCX). A C18 column was used with acetonitrile and water as mobile phases in a gradient elution. Ionization was performed using an electrospray positive ion source (ESI⁺), and detection was achieved by MS/MS in multiple reaction monitoring (MRM) mode. The linearity for carbendazim was good in the range of 0.5-50.0 μg/L; the linear equation was y=0.19988x+0.01842; and the correlation coefficient (r²) was 0.9985. The limit of detection (LOD) and limit of quantification (LOQ) were 0.25 μg/kg and 0.50 μg/kg, respectively. At spiked levels of 0.5, 1.0, 5.0, and 50.0 μg/kg, the recoveries ranged from 83.9% to 105.5%, and the relative standard deviation ranged from 1.1% to 3.2%. This method is simple and effective for the determination of carbendazim residues in P. clarkii.

Key words: solid phase extraction (SPE), high performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS), carbendazim, Procambarus clarkii

LI Yameng, GAN Jinhua, LI Jincheng, WU Lidong, LI Qin, XIAO Yushi, PENG Jie, CHEN Jianwu, LIU Huan. Determination of carbendazim residues in Procambarus clarkii by high performance liquid chromatography-triple quadrupole mass spectrometry[J]. Chinese Journal of Chromatography, 2020, 38(5): 611-616.

Figures/Tables 6

Table 1 Monitoring ion pairs (m/z), declustering potentials (DP) and collision energies (CE) of carbendazim and carbendazim-D4

Compound	Parent ion (m/z)	Product ion (m/z)	DP/V	CE/V
^*Quantitative ion.
Carbendazim	192.1	160.1^*	84	26
	192.1	132.1	84	40
Carbendazim-D4	196.0	164.0^*	84	28
	196.0	136.1	84	42

Fig. 1 Chromatograms of the standard solutions of carbendazim and carbendazim-D4

Fig. 2 Effect of different purification materials on the recoveries of carbendazim in Procambarus clarkii (n=6) PSA: primary secondary amine; GCB: graphitized carbon black; MCX: mixed-mode cation exchange solid phase extraction column.

Table 2 Recoveries of carbendazim in Procambarus clarkii eluted with different volume percentages of ammonium hydroxide-methanol mixture (n=6)

φ(Ammonium hydroxide)/%	Recovery/%	RSD/%
6	89.35	4.17
8	94.23	3.47
10	88.03	6.06

Fig. 3 Chromatograms of spiked Procambarus clarkii samples

Table 3 Recoveries and precisions of carbendazim in procambarus clarkii (n=6)

Tissue	Spiked level/(μg/kg)	Recovery/%	RSD/%
Muscle	0.5	83.9	1.5
	1.0	105.5	3.2
	5.0	94.6	1.1
	50.0	95.2	2.5

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22	GB 2763-2019

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