Determination Of Nicotine Residues In Foodstuffs By HPLC-MS/MS And GC-MS/MS

Nicotine is a kind of biology pesticides, with safty, high efficiency, and wide broadspectrum of antibiosis, however, when it entering the human body, it will have negative effect onthe people, lethal dose of people is50to70mg. In August2008, China’s output of bacteriaEuropean Union were found nicotine in cows liver, which results a lot of goods stranded wharfand and export enterprise suffer great losses. So China as the agricultural products exportingcountries must be strict on quality, and set up a set of feasible analysis method of nicotine.This research first optimized extraction conditions, concentration, purification conditions.Compared with the common extraction solven, the result show that there was no was nodifference when using eight kinds of solvent, such as5%NaOH (W/V)、2%formic acid (V/V)、water、methanol, acetone、2%formic acid methanol(V/V)、acetonitrile、ethyl acetate and so on.Compared with acid and alkaline enrichment instrument, the results showed that enrichmentprocess must be in acid conditions, and the Multivapor shows the best effect; evaporationPurification process using cation exchange solid-phase extraction (MCX) SPE small column inpurifying column, on conditions, with liquid product research are, the results show that with2%formic of samples, in aqueous solution was10mL5%of ammoniation methanol as eluentexhibit best eluent effect.To study the detection method of nicotine, liquid chromatography-mass spectrum/massspectrometry (HPLC-MS/MS) and gas chromatography/mass spectrometry/mass spectrometry(GC-MS/MS) were used in this experiment. Adopted HILIC column, the detection usingacetonitrile and acetic acid amine as gradient elution, and choosing ion scan (MRM) mode,163.0>130.1,163.0>117.1ion for detection, in optimized HPLC-MS/MS conditions, themethod of detection limit is:5ng/mL, the linear range is:5ng/mL to1000ng/mL. Using quartzcapillary column DB-17MS, temperature programing mode, choosing162>84,133>118fortesting ions, in GC–MS/MS conditions, detection limit of the method is:10ng/mL, the linearrange is between10ng/mL to1000ng/mL.Determination of nicotine residue in food was established by liquid chromatography-massspectrometry/mass spectrometry (LC-MS/MS) and gas chromatography-mass spectrometry/mass spectrometry (GC-MS/MS) in this study. Different solvent extraction were selectdepending on different sample matrix, the sample was purificated by the MCX solid phaseextraction column, using liquid quadrupole mass spectrometer and gas Quadrupole mass spectrometer in this measurement, quantitatived by externalstandard method. The limit ofdetection of LC-MS/MS are as follows:5μg/kg for Boletus, Morchella esculenta, drymushrooms, tea, edible fungus, honey, eggs,2.5μg/kg pork carrots,1μg/kg for broccoli andfresh fruit and vegetables, recovery range is between70%to110%, and the coefficient ofvariation is2.5%to10.2%. And the limit of detection of GC-MS/MS are as follows:10μg/kgfor dry mushrooms, tea, dehydration Onions, edible fungus, honey, eggs, pork,4μg/kg forcarrots, broccoli, tomato and fresh fruit and vegetables, recovery range is between70%to110%,and the coefficient of variation is1.13%-12.5%. This method with a simple pretreatment isexercisable, and suitable for the determination of food in nicotine residues, so it is very valuablein the determination of import and export food.