Chinese medicines are the drugs made from raw herbs based on the theory of traditional Chinese medicine.They are believed to be safer and healthier than synthetic drugs because of its natural ingredients.However,some criminals adulterate illegal chemical in Chinese medicines for pursuing illegal economic interests.There's no doubt that the behavior violates relevant rules and also causes great harm to patients and public security,hinders the development of Chinese medicine industry.In recent years,different doses of various drugs are added.Developing the detection methods has important practical significance.Antibiotics and glucocorticoids have often been added to Chinese medicines,because of the pharmacological characteristics.It is worth noting that these drugs hold a series of adverse side effects and even cause irreversible damage,especially in the absence of monitoring.Meanwhile,the added chemicals are also variety and possess similar chemical structures.Therefore,we need to develop one-time and fast detection method,realizing the high sensitivity,selectivity and accuracy analysis of multiple chemical structure.Establishing a new method for detecting added antibiotics and glucocorticoids will provide a more powerful technical support.Researchers have reported many technologies to detect the illegally added antibiotics and glucocorticoids.High performance liquid chromatography(HPLC),and chromatography-mass spectrometry(LC-MS)are widely used.HPLC method,however,need reference substance,can not analyze unknown additives which limit its application.LC-MS technology,combines high separation of chromatography and high identification ability of mass spectrometry,can realize the accurate quantitative and qualitative analysis of complex mixture.But the analyzers are low resolution mass spectrometry which can not provide much higher mass accuracy and not optimal for detecting a wide range of illegal added antibiotics and glucocorticoids.Orbitrap is one of the newest HRMS analyzers.It combines high speed with excellent quantification properties,offering an incomparable mass accuracy.In this study,we applied Q-Orbitrap HRMS to detect the illegal added antibiotics and glucocorticoids.The speed,accuracy and sensitivity are all improved.In this study,we applied the Q-Orbitrap high resolution mass spectrometry to the detection of illegal adulterated antibiotics and glucocorticoids in herbal medicines.The detection speed,accuracy and sensitivity are improved.We also established relevant databases about the detected chemicals.We mainly completed the following three parts:(1)We developed Q-Orbitrap high resolution mass spectrometry for the qualitative analysis of 9 cephalosporins,got fast(5 minutes),high accurate qualitative(resolution 70 000 FWHM)detection method.The method was applied to the detection of 14 batches of herbal medicines and cefalexin was detedted.(2)We developed Q-Orbitrap high resolution mass spectrometry for the qualitative and quantitative of 14 glucocorticoids in herbal medicines,got rapid(15min),selective(70 000 FWHM)and sensitive(LOD:1.0 ng/mL)detection method.The method was applied to the detection of 42 batches of herbal medicines and prednisone,prednisone acetate and cortisone acetate were detected.(3)We sorted out data and establish relevant databases about the detected chemicals.The establishment of the screening methods and database realizes targetless screening,which will help find more illegal additions,and provide technical support for combating illegal behavior. |