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LC-MS/MS method optimization and validation for trace-level analysis of 71 crop protection chemicals in pulses

  • Banerjee, Tirthankar1
  • Gupta, Suman1
  • Singh, Bijendra1
  • Narayanan, Neethu1
  • 1 ICAR-Indian Agricultural Research Institute, Division of Agricultural Chemicals, New Delhi, 110 012, India , New Delhi (India)
Published Article
Environmental Monitoring and Assessment
Publication Date
Oct 24, 2019
DOI: 10.1007/s10661-019-7859-4
Springer Nature


An analytical method involving modified QuEChERS (quick, easy, cheap, effective, rugged and safe) technique coupled with LC-MS/MS (liquid chromatography-tandem mass spectroscopy) has been developed for simultaneous identification and quantification of 71 pesticides (insecticides/acaricides/nematicides (32), fungicides (12), herbicides (26), plant growth regulator (1)) in different pulses (edible seeds of leguminous plants), namely gram, lentil, black gram and pea. The analysis was done using Shimadzu LC-MS/MS-8030 instrument equipped with Zorbax Eclipse Plus C-18 column operating under electrospray ionization (ESI) in positive and negative modes. Validation of method was done as per a single laboratory validation approach. Nine-point linear calibration curves for each pesticide were obtained in the range of 0.005 to 2 μg/g with correlation coefficient of ≥ 0.98. Limit of detection (LOD) for all the pesticides was achieved in the range of 0.001–0.015 μg/g, whereas the limit of quantification (LOQ) were found in the range of 0.01–0.05 μg/g. Recovery studies were conducted at 0.01- and 0.05-μg/g level of fortification using modified buffered QuEChERS method standardized for low moisture foods. It was observed that due to matrix interference, only around 75% of the pesticides were recovered in an acceptable range of 70–120% when compared against the solvent standard. With matrix-matched standards, 95% of the recovery results came within acceptable range with highly acceptable HorRat ratio (between 0.2 and 0.8) indicating satisfactory precision. The global and expanded uncertainties for estimation of each pesticide in above-mentioned pulse matrices were calculated to evaluate the suitability of the developed method for quantification of pesticides in pulse matrices.

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