Simultaneous Determination of 44 Pesticides in Tobacco by UPLC/MS/MS and a Modified QuEChERS Procedure

Abstract

A novel, simple, and rapid method for determination of the residues of 44 commonly used pesticides in tobacco was developed based on modified Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) procedures. The pesticides were extracted with acetonitrile and purified on a mixed sorbents column of primary secondary amine, C18, and graphitized carbon black. Quantitative determination of all pesticides was performed by ultra-performance LC/MS/MS in the positive or negative ionization mode by a single run due to the fast polarity switching capability of the mass spectrometer. Two precursor-product ion transitions were monitored for each compound in the multiple reaction monitoring mode. Quantification was carried out using matrix-matched standard calibration. The method has been validated by various tobacco cultivars, such as Burley, Oriental, and Virginia from different countries. Recoveries of the proposed method for spiked samples ranged from 71.1 to 109.8%, and RSD values were below 10%. The LOQ values were are all below the guidance residue levels proposed by the Agrochemical Advisory Committee of Cooperation Center for Scientific Research Relative to Tobacco. This method is valuable for measurement of pesticide residues in tobacco for QC and monitoring.

Magnetic graphene as modified quick, easy, cheap, effective, rugged and safe adsorbent for the determination of organochlorine pesticide residues in tobacco

“…Through calculation and investigation, the cost in clean-up step for one sample were $2.24 and less than $0.64 for traditional QuEChERS method [39] and the proposed QuEChERS method, respectively. What's more, the centrifugation or filtration step which was used in traditional QuEChERS method containing GCB or C18 was omitted in the proposed method [18,19,21,22,36], so it has the advantages of simplicity and rapidity. In whole, compared to other methods for the determination of OCPs in tobacco [22], water [29,[32][33][34][35], fruit and vegetable samples [36], the method in this study has the advantages of simple to operate, low cost and high clean-up ability.…”

“…Compared to the other sample preparation techniques such as LLE and PLE, QuEChERS technique shows not only good recoveries and relative standard deviations (RSDs) values in real samples, but higher and more consistent recoveries of targeted analytes than LLE and PLE [8]. So it has attracted much attention since its report [19][20][21][22]. The conventional QuEChERS technique involves an initial extraction with acetonitrile, followed by extraction/partitioning process with the addition of sodium chloride and anhydrous magnesium sulfate, then the extract is cleaned up by dispersive solid phase extraction with primary secondary amine (PSA) absorbent.…”

“…The conventional QuEChERS technique involves an initial extraction with acetonitrile, followed by extraction/partitioning process with the addition of sodium chloride and anhydrous magnesium sulfate, then the extract is cleaned up by dispersive solid phase extraction with primary secondary amine (PSA) absorbent. In recent years, the QuEChERS technique has been widely applied for the determination of pesticide residues in tobacco with minor modifications [21,22]. However, centrifugation or filtration procedure is essential to separate the absorbents from extract in those reports, which is a little troublesome and tedious [23,24].…”

Rapid and sensitive multiresidue analysis of pesticides in tobacco using low pressure and traditional gas chromatography tandem mass spectrometry

“…Table 1 presents comparative evaluation of some reported multiresidue methods in tobacco. These methods mostly involve sample preparation by QuEChERS technique with some modifications [9][10][11] and also ethyl acetate based extraction [4]. The reported instrumentation techniques include GC [12,13], GC-MS [3,4], two-dimensional GC with time-of-flight mass spectrometry (GC × GC-TOFMS) [14], and GC-MS/MS [11,15,16] with traditional GC hardware set-up targeting selective number of pesticides (varying from 10 to 159 compounds) with chromatographic run times ranging from 18.67 to 55.1 min.…”

Simultaneous determination of 223 pesticides in tobacco by GC with simultaneous electron capture and nitrogen-phosphorous detection and mass spectrometric confirmation

“…Several miniaturized methods have been introduced, e.g. matrix solid phase dispersion MSPD [16] and QuEChERS (quick, easy, cheap, effective, rugged, and safe) [17][18][19] which eliminate most of the complications of classical extraction.…”