Improved analysis of folpet and captan in foods using liquid chromatography-triple quadrupole linear ion trap mass spectrometry: applying mass filtering, collision, and trapping conditions

Accurate and highly sensitive analysis of folpet and captan was accomplished using liquid chromatography-triple quadrupole linear ion trap mass spectrometry (LC-QqQIT) with selective ion mode; mass filtering, collision, and trapping condition. Dimensional mass spectrometry (MS3) parameters were optimized for the residue detection of folpet and captan in six food commodities (apples, tomatoes, sweet pepper, wheat flour, sesame seeds, and fennel seeds). The sample preparation method was based on the known QuEChERS protocol, except a mixture of acetonitrile/acetone was used for the sample extraction from the sesame seeds. The robustness and reliability of the developed MS3 method were demonstrated by performing a full validation, according to SANTE/11312/2021, at 0.01-0.25 mg/kg. Recovery ranged from 83 to 118% with a relative standard deviation below 19% in all the tested commodities, and limits of quantifications (LOQs) were 0.01 mg/kg in apples and tomatoes; 0.03 mg/kg in sweet pepper; and 0.05 mg/kg in wheat flour, sesame seeds, and fennel seeds. Monitoring results showed that about 90% of apples contained captan residue, and in sweet pepper, concentrations of captan and folpet as high as 1.57 and 0.97 mg/kg were found, respectively. The novel developed MS3 method enabled more reliable identification of these commonly problematic fungicides at lower LOQs than previously reported methods.

Automated summary

Accurate and highly sensitive analysis of folpet and captan was achieved using LC-QqQIT with a selective ion mode and optimized MS3 parameters. The developed method showed robustness and reliability through full validation, yielding recovery rates from 83 to 118% and LOQs ranging from 0.01 to 0.05 mg/kg in various food commodities. Monitoring results revealed the presence of captan residue in approximately 90% of apples and high concentrations of captan and folpet in sweet pepper. The novel MS3 method enables more reliable identification of these fungicides at lower LOQs compared to previous methods.