The Application Of Uhplc Ms/ms In The Determination Of Illegally Adulterating Compounds In Food

Background The health food for improving gastrointestinal function are at high risk of illegally adulterating chemical drugs, which may be added the following categories of chemical drugs: 1) laxatives such as phenolphthalein, bisacodyl; 2) weight loss drugs such as sibutramine, fenfluramine; 3) drugs strengthening gastrointestinal motility such as domperidone, cisapride, mosapride; 4) drugs which can anti acid and protect gastric mucosal such as cimetidine, ranitidine, rebamipide. These chemical drugs are prescription drugs, need to be taken under the guidance of doctors because of certain poisonous and side effects, misusing of these chemical drugs will lead to serious consequences or even life-threatening. The industrial dyes illegally adulterated in hotpot condiment contain basic orange2, basic orange 21, basic orange 22, acid orange A, auramine 0, crystal violet. It’s forbidden to add these dyes to the food for all these having different degrees of harm to human body. There was no reported method can be used to simultaneously,rapidly andaccurately determine these two kinds of illegally adulterated compounds.Objective To establish an UHPLC-MS/MS method and a QTOF-MS method for simultaneous determination of 10 compounds illegally adulterated in Health food for improving gastrointestinal function, and establish an UHPLC-MS/MS method for simultaneous determination of 6 Industrial dyes illegally adulterated in hotpot condiment.Methods The separation and analysis was performed on a Zorbax SB C18 column(2.1 mm×100 mm,1.8 μm). The mobile phase consisted of 0.1 % acetic acid containing 20 mmol.L-1 ammonium acetate and methanol(Gradient elution). The column temperature was set at 35 ℃ with flow rate of 0.2 m L?min-1.Electrospray ionization(ESI) source was applied and operated in the positive mode. Multiple reaction monitoring(MRM) mode was used to quantify the 10 compounds illegally adulterated in health food for improving gastrointestinal function. The separation and analysis was performed on a Waters Atlantis d C18 column(2.1×100 mm,1.8 μm). The mobile phase consisted of 0.1 % acetic acid containing 10 mmol.L-1 ammonium acetate and acetonitrile(Gradient elution). The column temperature was set at 35 ℃ with flow rate of 0.2 m L?min-1.Electrospray ionization(ESI) source was applied and operated in the positive and negative modes. Multiple reaction monitoring(MRM) mode was used to quantify the 6 Industrial dyes illegally adulterated in hotpot condiment.Results The assay linearities of the 10 compounds illegally adulterated was confirmed over 1~250 times of the limit of quantification. The average recoveries( n= 15) were 86.9 %-112.8 % and the detection limits were 0.02~0.4 ng.m L-1. The relative standard deviation was less than 5 %(n=6). Totally 4 positive samples in the 40 batches of health food were detected. The relative standard deviation was less than 4.2 ppm between the molecular of 10 compounds illegally adulterated measured on QTOF-MS and the molecular of theory. The assay linearities of the 6 Industrial dyes illegally adulterated was confirmed over 1~50 times of the limit of quantification. The average recoveries( n= 15) were 82.5 %-117 % and the detection limits were 0.17~2.54 ng.m L-1. The relative standard deviation was less than 5.8 %(n=6). Totally 1 positive samples in the 40 batches of hotpot condiment were detected.Conclusion The established methods can be used to determine 10 compounds illegally adulterated in Health food for improving gastrointestinal function and 6 Industrial dyes illegally adulterated in hotpot condiment.