| Since the end of 20 th, Adulterating became a new counterfeiters way in healthy products, which posed potential threat for human health and disturbed the social order. At present, a large number of analytical methods have been proposed by Liquid chromatography. However, they were only appropriate for several targeted compounds. Therefore, it is necessary to develop a rapid analytical method for determining multi-additives at the same time. Column is an important part of Liquid chromatography. Sub-3μm particle column was developed aiming at retaining column efficiency and requring relatively low pressure drop. Comparing to the porous sub-2μm particle column, it could achieved similar efficiency separations. Meanwhile the low back pressures allows to be most widely employed on the high performance lquid chromatography systems.Therefore, this study focused on these aspects, the traditional Chinese medicines, health care foods, Chinese herbs and foods will be selected as representatives research objects, to established the rapid determination method by sub-3μm chromatographic technique. The main research contents and results were as follows:In the first chapter, the status, hazard and characteristic of adulteration and analytical methodologies of health products and the development of column have been summarized. Application prospects of common techniques and sub-3μm chromatographic technique on rapid determination of adulterants.In the second chapter, a method for simultaneous rapid determination 18 adulterants in traditional Chinese medicines of promoting sexual enhancement was developed by high performance liquid chromatography(HPLC) and liquid chromatography-tandem mass spectrometry(LC-MS/MS). The results indicated determination of 18 adulterants within 18 minutes. The linear range, average recoveries, and precision of 18 drugs could fully meet all the requirements of qualitative and quantitative analysis. The method was verified by applying it to 101 different samples, and 7 kinds of drugs and an unknown sildenafil analogue were detected. The adulterated was proved to be 5-{5-[4-2(-hydroxyethyl)piperazin)piperazin)sulfony]-2-propoxyphenyl}-1-methy-3-propyl-1H-pyrazolo[4,3d]pyrimidine-7(6H)-thione by thin layer chromatography(TLC), column chromatography(CC) and HPLC for separation and purification, and Nuclear magnetic resonance(NMR) and mass spectrometry(MS) for the determination of the chemical structure.In the third chapter, a method was developed for determination and conformation of 21 antihypertensive chemical drugs in health foods by HPLC and LC-MS/MS. The results indicated determination of 21 analytes within 17 minutes. The linear range, average recoveries, and precision of 21 drugs could fully meet all the requirements of qualitative and quantitative analysis. The applicability method was verified by applying to 107 real health care food samples, and neigh drugs and an unknown drugs were detected. It was proved varstan by LC-MS/MS.In the fourth chapter, a method for simultaneous rapid determination 37 synthetic colorants in meat product was developed by HPLC and LC-MS/MS. The results indicated determination of 25 water-soluble colors and 12 fat-soluble colors within 16 minutes. The samples were extracted by the sequential extraction. Then the extraction solution was purified by solid phase extraction(SPE) and dispersed solid phase extraction(DSPE). The linear range, average recoveries, and precision of 37 colors could fully meet all the requirements of qualitative and quantitative analysis. The applicability method was verified by applying it to 200 different meat products, and six synthetic colorants were detected.In the fifth chapter, a rapid method was developed for determination of 12 yellow pigments in illegally dyed pangolin by HPLC and LC-MS/MS. The results indicated determination of 12 yellow colors within 16 minutes. The linear range, average recoveries, and precision of 12 yellow colors could fully meet all the requirements of qualitative and quantitative analysis. The applicability method was verified by applying it to 60 different pangolin samples, and a yellow pigment was detected, which was proved gardenia yellow with LC-MS/MS.In the six chapter, the research work was summarized with three innovations. In this work, it is the first time at home and abroad to establish a rapid analytical method for determining multi-additives at the same time by the sub-3μm chromatographic technique. As a novel pretreatment technology, Qu ECh ERS(Quick, Easy, Effective, Rugged and Safe) was been utilized in analysis of fat- soluble colors. Three unknown adulterants were detected and descried in real samples.In conclusion, the develop rapid determination methods with sub-3μm chromatographic technique were quick, effective, sensitive and reliable for the analysis of adulterants in healthy products. It could provide a powerful tool for the quantification and confirmation of anti-adulteration... |
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