Evaluation of GC-ICP-MS/MS as a New Strategy for Specific Heteroatom Detection of Phosphorus, Sulfur, and Chlorine Determination in Foods

Abstract

For the first time in the literature, application of a GC-ICP-MS/MS method for the selective and sensitive detection of specific heteroatoms of phosphorus, sulfur, and chlorine has been accomplished. As a proof of concept, organophosphorus, organosulfur, and organochlorine pesticides in various food matrices have been studied. For the detection of organophosphorus and organosulfur pesticides, oxygen was used in the collision reaction cell (CRC) to convert P (m/z 31) to PO(+) (m/z 47) and S (m/z 32) to SO(+) (m/z 48). Similarly, ClH2(+) (m/z 37) was monitored after the reaction of Cl (m/z 35) with hydrogen in the CRC for the determination of organochlorine pesticides. Real food samples (baby food purees, fresh vegetables, loose tea) were screened for their pesticide content, following preparation of triplicate extracts using QuEChERS (quick, easy, cheap, effective, rugged, and safe). Excellent linearity with correlation coefficients R ≥ 0.997 was achieved, and the lowest detection limits obtained for the organophosphorus, organosulfur, and organochlorine pesticides were 0.0005, 0.675, and 0.144 μg/kg, respectively.

Quantification of Glyphosate and AMPA by HPLC-ICP-MS/MS and HPLC-DAD: A Comparative Study

“…19 Different gases such as helium, hydrogen, oxygen and ammonia could be used in CRC, 31 but O 2 was chosen in this study because it was verified in some studies that the reaction with oxygen is thermodynamically favorable and there is a significant increase of sensitivity in detecting phosphorous compounds in food matrices and water. 20,23 A recent study also obtained better results using oxygen gas for detecting organophosphorus pollutants in water. 32 The comparison of these analytical parameters showed that both methods were selective, but the method using ICP-MS/MS as the detector presented a four times shorter analysis time and a cleaner chromatogram.…”

“…The ICP-MS/MS has been used to determine the heteroatoms instead of compounds, i.e., to determine phosphorus in the glyphosate and AMPA molecules. 20 Moreover, the use of the MS/MS mode eliminates interferences from the matrix, thereby increasing the technique's sensitivity. 21 The aim of the present work was to compare two detection systems coupled to HPLC in quantifying glyphosate and AMPA, evaluating analytical performance through selectivity, linearity, limit of detection, analysis and sample preparation time.…”

“…The O 2 was introduced as reaction gas in the CRC, and the second quadrupole was adjusted to monitor the reaction product m/z 47 ( 31 P 16 O + ), so that these ions were detected with minimal interference: 20 31 P + + 16 O 2 → 31 P 16 O + + 16 O ΔH reaction = −3.17 eV 1The analytical conditions were: ZORBAX SB-C8 (4.6 × 150 mm, 5 μm), injection volume 50 μL, mobile phase composed of 50 mM acetic acid/ammonium acetate solution: 5 mM tetrabutylammonium: 1% methanol with pH = 4.7, isocratic elution with 1.0 mL min −1 . 23 The HPLC-ICP-MS/MS analysis conditions are summarized in Table 1.…”

Emerging techniques for determining the quality and safety of tea products: A review

“…The application of a GC‐ICP‐MS/MS method (Nelson et al., 2015) for the selective and sensitive detection of specific heteroatoms of phosphorus, sulfur, and chlorine has been accomplished, and commercial tea (leaf) as well as other food samples (baby food purees and fresh vegetables) are screened for its pesticide contents, following the preparation of triplicate extracts using QuEChERS. The correlation coefficient R of this application was greater or equal to 0.997, and the lowest LODs of the organophosphorus, organosulfur, and organochlorine pesticides were 0.0005, 0.675, and 0.144 µg/kg, respectively.…”

Inductively coupled plasma – Tandem mass spectrometry (ICP-MS/MS): A powerful and universal tool for the interference-free determination of (ultra)trace elements – A tutorial review

“…Very recently, the H2-addition mass shift reaction for Cl was also used by Nelson et al [45] in the development of a GC-ICP-MS/MS method for the detection of organochlorine pesticides in food matrices, where extremely low detection limits are desirable.…”