Amantadine‐functionalized magnetic microspheres and stable isotope labeled internal standards for reducing matrix effect in determination of five opium alkaloids by liquid chromatography‐quadrupole linear ion trap mass spectrometry

Abstract

Amantadine-functionalized magnetic microspheres (Fe 3 O 4 @SiO 2 @ADME) were prepared and applied as magnetic solid-phase extraction (MSPE) adsorbents for the enrichment and analysis of five opium alkaloids in hotpot seasoning samples with liquid chromatography coupled to quadrupole linear ion trap mass spectrometry (LC-QqQ LIT -MS/MS). The adsorbents could strongly adsorb the opium alkaloids via hydrogen-bonding, hydrophobic, and π-π conjugation effects. The established MSPE, combined with stable isotope-labeled internal standards could reduce the matrix effect significantly. In the LC-QqQ LIT -MS/MS analysis, the precursor and product ions of the analytes were monitored quantitatively and qualitatively by the multiple reaction monitoring and enhanced product ion mode, improving the reliability of detection for real samples. Under the optimum conditions, the limits of detection and limits of quantification were found to be in the range of 0.05-0.8 μg/ kg and 0.25-2.5 μg/kg, respectively, and the recoveries of all targets were in the range 80.1-115.3%, with the intra-day and inter-day relative standard deviations being less than 9.4 and 10.7%, respectively. Finally, the proposed method was successfully applied to the determination of illegal additives of opium alkaloids in hotpot seasoning samples. K E Y W O R D Smagnetic solid-phase extraction, liquid chromatography coupled to triple quadrupole linear-ion trap tandem mass spectrometry, opium alkaloids, matrix effect

Mesostructured Silica-Coated Magnetic Nanoparticles to Extract Six Opium Alkaloids in Poppy Seeds Prior to Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry Analysis

“…To perform this, the amount of CTAB present in the materials was monitored after the removal treatment by using FT-IR spectroscopy before the functionalisation process by checking the presence of the bands of the -CH 2 and -CH 3 groups from CTAB at 2855 cm −1 and 2925 cm −1 , respectively. The first treatment was performed with a Soxhlet acetone extraction, as in most studies [ 22 , 23 , 36 , 37 ]. However, the intensity of these bands was remarkable ( Figure S3a , spectrum 2), which showed that this treatment was not effective in eliminating the surfactant.…”

“…As has been observed, the most used separation technique is HPLC, although there are authors who also use UHPLC because it has the advantage of reducing analysis times. Chromatography times for methods developed with HPLC-MS/MS are between 15 and 30 min [ 6 , 20 ], while methods developed with UHPLC-MS/MS take between 7 and 10 min [ 1 , 22 ]. A noteworthy aspect of this proposed method is that only 5 min were sufficient to efficiently quantify the six opium alkaloids, which is considerably less time than the methods already developed to quantify opioids in the literature.…”

“…MSPE consists of dispersing the magnetic material in a solution with the sample for a few minutes. Once it is in equilibrium, it is recovered with the help of a magnetic field and, finally, the analytes are desorbed which can avoid tedious filtration, centrifugation or sedimentation steps [ 22 ]. Adsorbent material type is an important parameter in MSPE procedure because it will determine the ability to purify the samples.…”

“…Adsorbent material type is an important parameter in MSPE procedure because it will determine the ability to purify the samples. Until now, Fe 3 O 4 particles covered with amorphous silica are the most used as a magnetic adsorbent, which can be functionalised with different organic groups as natural polymers or graphene [ 22 , 23 , 24 , 25 ]. However, the use of mesostructured silica is increasingly important because of their larger surface area, which can bind more of the functional groups and their uniform porous structure can facilitate access to the analytes [ 26 , 27 ].…”

New Validated Method for the Determination of Six Opium Alkaloids in Poppy Seed-Containing Bakery Products by High-Performance Liquid Chromatography-Tandem Mass Spectrometry after Magnetic Solid-Phase Extraction

“…This technique is equipped with a triple quadrupole (TQ) detector with electrospray ionization in the positive mode (ESI+) and multiple reaction monitoring (MRM) for multiple analyte detection. ,,,− Regarding sample treatment, until now, solid–liquid extraction (SLE) of OAs from poppy seeds has been performed in most studies. ,,, However, it is essential to carry out an adequate sample treatment that includes a preconcentration and/or purification step to eliminate the possible matrix effects, thus avoiding erroneous results and extending the useful life of the chromatographic column and MS detector. For this reason, a solid-phase extraction (SPE) step is used in some studies. ,,− In addition, the magnetic dispersive SPE (MSPE) version has also been evaluated for this task ,− as the sorbent material can be quickly separated from the solution by using an external magnetic field, instead of filtration or high-speed centrifugation as required in common dispersive SPE. Then, MSPE is a simpler, faster, easily miniaturized, and environmentally friendly preconcentration/purification technique .…”