Journal
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
Volume 54, Issue 6, Pages 2012-2017Publisher
AMER CHEMICAL SOC
DOI: 10.1021/jf052897v
Keywords
perchlorate; ion chromatography; mass spectrometry; sample preparation; internal standard; extraction; ion suppression; plants; lettuce; spinach; vegetables; Lactuca sativa L.; Spinacia oleracea L.
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A sample preparation method was developed to quantify environmentally relevant (low micrograms per liter) concentrations of perchlorate (CIO4-) in leafy vegetables using IC-ESI-MS. Lettuce and spinach were macerated, centrifuged, and filtered, and the aqueous extracts were rendered water-clear using a one-step solid-phase extraction method. Total time for extraction and sample preparation was 6 h. Ion suppression was demonstrated and was likely due to unknown organics still present in the extract solution after cleanup. However, this interference was readily eliminated using a (ClO4)-O-18-internal standard at 1 mu g/L in all standards and samples. Hydroponically grown perchlorate-free butterhead lettuce was spiked to either 10.3 or 37.7 mu g/kg of fresh weight (FW), and recoveries were between 91 and 98% and between 93 and 101%, respectively. Five types of lettuce and spinach from a local grocery store were then analyzed; they contained from 0.6 to 6.4 mu g/kg of FW. Spike recoveries using the store-bought samples ranged from 89 to 100%. The method detection limit for perchlorate in plant extracts is 40 ng/L, and the corresponding minimum reporting limit is 200 ng/L or 0.8 mu g/kg of FW.
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