Quantitation and Dietary Risk Assessment of Hexazinone Residue in Blueberry Fruit

Abstract

In order to determine the residue of hexazinone in blueberry fruit, field experiments in Zhejiang, Jilin, Liaoning and Beijing, China were conducted using 75% hexazinone water dispersible granules. An analytical method was established for determining residual hexazinone in blueberry fruit utilizing ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with an electrospray ionization source in the positive ion mode (ESI+). The samples were extracted with acetonitrile while vortexing, salted out, and then purified on a column packed with primary secondary amine (PSA) and C18 before measurement. The linearity, matrix effect, limit of quantification (LOQ), trueness (recovery rate) and precision (relative standard deviation (RSD)) of the proposed method were studied. Good linearity (r > 0.999 8) was found in the concentration range from 0.000 1 to 0.01 mg/L. The matrix effect was −7.7%. The LOQ was 0.01 mg/kg. The average recovery of hexazinone from blueberry fruit at spiked concentration levels of 0.01, 0.1 and 1.0 mg/kg ranged from 87% to 91%, with a RSD less than 3.7%. The field experiments showed that the residual level of hexazinone in blueberry fruit was below 0.01 mg/kg at 90 and 100 days after application, which was lower than the maximum residue limits (MRL) established in the US, Japan and South Korea (0.6, 0.2 and 0.05 mg/kg, respectively). The results of chronic dietary risk assessment showed that the estimated daily intake of hexazinone for general populations was 0.002 2 mg. The dietary risk quotient (RQ) was only 0.084%, indicating a low risk of dietary hexazinone intake. Therefore, it is recommended that 75% hexazinone water dispersible granules (WG) be applied in a single dose up to 1 800 g/hm2 to blueberry orchards; the pre-harvest interval (PHI) be 90 days.

Keywords

• hexazinone; blueberry fruit; residue; dietary risk assessment