Most toxins are water soluble (along with other crap) so HPLC would be my 1st choice. However, you need a 'very' sensitive detector like MS/MS (not just MS)!
Souptik Bhattacharya I wanted to do ELISA, but it was very troublesome to prepare HRP conjugated nanobody. ELISA is the best but I am looking for something else.
With GS-MS the toxin must be volatile (turn into a gas). The toxin can always be derivatized into a volatile ester (along with everything else in your sample matrix).