On-cartridge derivatisation using matrix solid phase dispersion for the determination of cyclamate in foods

- A novel method was developed for the determination of cyclamate in foods.
- On cartridge derivatisation, using matrix solid phase dispersion, was developed.
- A new derivatisation reaction for cyclamate conversion to 2-chlorocyclohexanone was developed.
- The method was rapid, simple, inexpensive, effective.

A novel method for determination of sodium cyclamate in foods was developed. In this method, a syringe was loaded with the homogeneous mixture of the sample, KMnO4 powder and silica dispersant and used as a matrix solid phase dispersion (MSPD) reactor. As the reactor was infiltrated with small amounts of concentrated HCl, cyclamate was converted to 2-chlorocyclohexanone quickly and effectively within 5 min and determined by HPLC on a reversed-phase column using UV detection at a wavelength of 310 nm. Comparing with the traditional derivatisation in solution, the better clean-up was provided using on-cartridge derivatisation of MSPD, and much time, labor, and expense were saved. The results showed good linearity (r2 = 0.9998) over the concentration range of 1-500 mg/L. The limit of detection (LOD) and limits of quantification (LOQ) of the cyclamate were 0.3 mg/L and 1 mg/L respectively. The recoveries ranged from 91.6% to 101.3% with the relative standard deviations (RSDs) in the range of 2.5%-4.3%.

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