Application And Study Of Electrospray Ionization-High Performance Ion Mobility Spectrometry In The Detection Of Illegally Added Substances In Traditional Chinese Medicine Materials

Problems are quite common in quality safety of traditional Chinese medicinal materials.Despite prohibitions concerned,dyeing,adulteration and weight gain still exist as the three key problems,among which the dyeing problem is the most serious.Substandard traditional Chinese medicinal materials exerts a direct influence in the effective treatment.Illegal addition of dyed material may even endanger the patient’s health,which will,on the one hand,trigger an array of public questions on traditional Chinese medicinal materials treatment,and on the other hand,hinder the sound development of the whole traditional Chinese medicine industry.Researches on working out a fast,efficient and convenient testing method to differentiate illegal dyeing additives from the medicinal materials is pretty urgent as well as important.Taking advantage of modern detection technology to fundamentally ensure the medicinal materials quality is an effective way to strengthen public medication safety.This thesis makes a qualitative and quantitative study on dyeing substances illegally added into the traditional medicinal materials by making full use of Electrospray Ionization-High Performance Ion Mobility Spectrometry with its easy operation,fast detection and high sensitivity.Its main research contents are as follows:1.A parameter database on IMS for the rapid and separate test on 12 kinds of dyeing substances including Sun Yellow,Lemon Yellow,Carmine,Auramine O,Sudan Ⅳ,Allura Red,OrangeⅡ,Amaranth,Indigo,Brilliant Blue,Acid Red 73 and Erythrosine B,and another parameter database on IMS for the rapid and simultaneous tests on 7 kinds of them are both established by analyzing the effects on dyeing substances test of IMS parameters such as ion source voltage,drift tube voltage,inlet temperature,drift tube temperature,injection liquid flow rate,drift gas flow rate,ion gate voltage and gate pulse width.Besides,the stability of testing method is examined.2.The thesis makes a study on IMS for the rapid and qualitative tests on Auramine O in each traditional Chinese medicinal materials including Typhae Pollen,Corydalis Rhizoma and Phellodendri Chinensis Cortex,and Orange II in each traditional Chinese medicinal materials including Carthami Flos,Schisandrae Chinensis Fructus and Corydalis Rhizoma.In addition to this,the matrix effect in each traditional Chinese medicinal materials and the minimum detected limits of Auramine O and Orange II are examined.3.Polyamide solid phase extraction-IMS for the qualitative and quantitative test on dyeing substances illegally added into the traditional Chinese medicinal materials are studied.Qualitative study refers to simultaneous test on 4 kinds of dyeing substances in Carthami Flos and Schisandrae Chinensis Fructus.Through the pretreatment of polyamide solid phase extraction to the traditional Chinese medicinal materials,almost no target substances are interfered by matrix peak,and the minimum detected limit of each dyeing substances in Schisandrae Chinensis Fructus is below 1 μg·ml-1,and the minimum detected limit of each dyeing substances in Carthami Flos is below 2 μg·ml-1.Quantitative study refers to the measurement on the contents of 4 kinds of dyeing substances in Carthami Flos.In order to measure accurately,extraction solvent and extraction time are examined,and several key factors including extraction solution pH,the amount of the solution of methanol-formic acid(6:4)and the amount of 2% ammoniated methanol solution are improved and optimized.After a systematic methodology verification,an accurate,effective and stable method of polyamide solid phase extraction-IMS for quantitative test on dyeing substances in Carthami Flos is figured out.4.Polyamide solid phase extraction-IMS for the qualitative test on dyeing substances in a random sample of Carthami Flos are studied.The results are verified by both HPLC method and LC-MS method.