Citation: CUI Zongyan, SUN Yang, GE Na, ZHANG Jinjie, LIU Yongming, LI Adan, CAO Yanzhong. Simultaneous determination of cyhexatin, triphenyltin and fenbutatin oxide residues in fruits and vegetables by Grignard derivatization and gas chromatography coupled to tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(8): 855-860. doi: 10.3724/SP.J.1123.2014.04031 shu

Simultaneous determination of cyhexatin, triphenyltin and fenbutatin oxide residues in fruits and vegetables by Grignard derivatization and gas chromatography coupled to tandem mass spectrometry

CUI Zongyan ¹ ,
SUN Yang ² ,
GE Na ¹ ,
ZHANG Jinjie ¹ ,
LIU Yongming ¹ ,
LI Adan ² ,
CAO Yanzhong ^1,,

1.
1. Qinhuangdao Entry-Exit Inspection and Quarantine Bureau, Qinhuangdao 066004, China;

Corresponding author: CAO Yanzhong,
Received Date: 18 April 2014
Available Online: 25 June 2014
Fund Project: 国家质检总局科技计划项目(2014IK090). (2014IK090)

A method for the simultaneous determination of cyhexatin, triphenyltin and fenbutatin oxide residues in fruits and vegetables was developed by Grignard derivatization and gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). The samples were firstly digested by HCl/THF (1:10, v/v), then extracted by hexane and followed by the derivatization with Grignard reagent (EtMgBr). Then after purification using florisil SPE columns, the sample extracts were finally analyzed by GC-MS/MS. The qualitative and quantitative determinations of the three organotin pesticides were performed by the tandem mass in multiple reaction monitoring (MRM) mode. By using apple as a representative matrix, the limits of detection (LODs) obtained by the proposed method for cyhexatin, triphenyltin and fenbutatin oxide were 2.0, 1.5 and 3.4 μg/kg (as Sn), respectively. The average recoveries for the three organotin pesticides were in the range of 72.4%-107.1% at the spiked levels of 10, 20, 50 and 200 μg/kg (as Sn) and the relative standard deviations (RSDs) ranged from 0.4% to 14.2%. The proposed method was validated to have good linearity, high sensitivity, selectivity and accuracy for the simultaneous determination of cyhexatin, triphenyltin and fenbutatin oxide in fruits and vegetables. The sensitivity of this method can meet the requirements of the inspection for the three organotin pesticides at the level of maximum residue limits (MRLs) set by China and some other countries.
- Grignard reagent,
- derivatization,
- gas chromatography-tandem mass spectrometry (GC-MS/MS),
- cyhexatin,
- triphenyltin,
- fenbutatin oxide,
- fruits,
- vegetables
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