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Development of rapid and simultaneous chromatography for the determination of 9 preservatives and 8 PAHs of safety concern in the food and oriental medicine industries

  • Jwahaeng Park (박좌행, 대학원 생명공학과 식품바이오전공)

초록/요약

This dissertation explores advanced analytical methods for safety management in both processed animal products and herbal medicines. The primary objective is to ensure product safety and regulatory compliance by optimizing and validating novel testing procedures. This research specifically aims to develop and validate rapid simultaneous chromatography methods for determining the presence of 9 preservatives and 8 PAHs, each recognized as safety concerns in the food and oriental medicine industries. The first objective was achieved through the development of a rapid and sensitive ultraperformance liquid chromatography (UPLC) method for the simultaneous determination of nine chemical preservatives in processed animal products. The UPLC method demonstrated high sensitivity and specificity, with limits of detection (LOD) and quantification (LOQ) for the preservatives ranging from 0.02 to 0.23 μg/g and 0.07 to 0.76 μg/g, respectively. The method also showed excellent precision, with relative standard deviations (RSD) for intraday and interday analyses ranging from 0.00 % to 2.93 % and 0.67 % to 5.37 %, respectively. The second objective involved optimizing and validating a gas chromatography-tandem mass spectrometry (GC-MS/MS) method for the detection of eight PAHs in herbal medicines. The GC-MS/MS method was successfully validated, with LODs and LOQs for the PAHs ranging from 0.09 to 0.37 μg/kg and 0.26 to 1.11 μg/kg, respectively. The method demonstrated high precision and accuracy, with recovery rates for the PAHs ranging from 54.7 % to 125.0 % and RSDs between 0.8 % and 22.3 %. Furthermore, the study compared the performance of the UPLC method with existing high-performance liquid chromatography (HPLC) techniques and found that UPLC offered significant improvements in speed, sensitivity, and accuracy. For PAH analysis, the study compared the GC-MS/MS method with existing sample preparation techniques, specifically replacing the traditional hexane-based liquid-liquid extraction with a new DFA extraction method using N, N-dimethylformamide/water mixture (9:1, v/v). The DFA method, tailored according to the presence of essential oils or starch grains, provided higher recovery rates and improved efficiency. The application of these validated methods to real-world samples demonstrated their practical utility in monitoring and ensuring compliance with safety standards. The detection of sorbic acid in 5.8 % of the processed animal product samples and various levels of PAHs in herbal medicine samples underscored the importance of continuous monitoring to protect consumer health. In conclusion, this dissertation has made significant contributions to the field of food and oriental medicine safety by providing advanced analytical methods that enhance the detection and monitoring of chemical contaminants. These methods will aid in ensuring product safety and regulatory compliance, ultimately benefiting public health.

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목차

TABLE OF CONTENTS
ABSTRACT ................................................................................................................... i
ABSTRACT IN KOREAN .............................................................................................. iii
PREFACE ...................................................................................................................... vii
ACKNOWLEDGMENTS .............................................................................................. viii
TABLE OF CONTENTS ................................................................................................ ix
LIST OF TABLES .......................................................................................................... xii
LIST OF FIGURES ........................................................................................................ xiv
CHAPTER 1. LITERATURE REVIEW ............................................................................ 1
1.1 Preservatives .......................................................................................................... 1
1.1.1 Previous work of analytical method for preservatives ................................... 1
1.1.2 Objective of this study for preservatives ......................................................... 2
1.2 Polycyclic aromatic hydrocarbons ....................................................................... 2
1.2.1 Herbal medicines.................................................................................................. 3
1.2.2 Previous work of analytical method for PAHs ................................................. 4
1.2.3 Objective of this study for PAHs ....................................................................... 4
1.3 Objective .................................................................................................................. 5
1.4 Organization of this dissertation .......................................................................... 5
CHAPTER 2. SIMULTANEOUS AND RAPID ANALYSIS OF PRESERVATIVES
IN PROCESSED ANIMAL PRODUCTS BY ULTRA-PERFORMANCE
LIQUID CHROMATOGRAPHY....................................................................................... 7
2.1 Materials and Methods ........................................................................................... 7
2.1.1 Food samples ........................................................................................................ 7
2.1.2 Standard preservatives and chemicals ............................................................ 7
2.1.3 Preparation of standard stock solution and working solution ....................... 7
2.1.4 Spiking recovery test ........................................................................................... 8
2.1.6 UPLC analysis ....................................................................................................... 8
2.1.7 HPLC analysis ........................................................................................................ 9
2.1.8 Statistical evaluation ............................................................................................. 9
2.2 Results and Discussion ............................................................................................ 9
2.2.1 Optimization of the mobile phase and gradient elution mode ......................... 9
2.2.2 Validation of the method....................................................................................... 10
2.2.3 Levels of chemical preservatives in processed animal products in a field
study ................................................................................................................................. 17
2.2.4 Discussion .............................................................................................................. 19
CHAPTER 3. GC-MS/MS METHOD FOR DETECTION OF POLYCYCLIC
AROMATIC HYDROCARBBONS IN HERBAL MEDICINES ........................................... 20
3.1 Materials and Methods ............................................................................................. 20
3.1.1 Chemicals and Reagents ....................................................................................... 20
3.1.2 Standard Solution Preparation ............................................................................. 20
3.1.3 Sample Preparation ............................................................................................... 21
3.1.4 Sample Extraction .................................................................................................. 24
3.1.5 Sample Purification ................................................................................................ 27
3.1.6 GC-MS/MS Analysis .............................................................................................. 27
3.1.7 Statistical Evaluations ............................................................................................ 28
3.1.8 Matrix Effect ............................................................................................................ 28
3.1.9 Method Validation ................................................................................................... 28
3.1.10 Monitoring of 8 PAHs in Herbal Medicine........................................................... 29
3.2 Result and Discussion ................................................................................................ 29
3.2.1 Optimization of the Analytical Method and Selection of HMs
Representatives ................................................................................................................ 29
3.2.2 Matrix Effect ............................................................................................................. 35
3.2.3 Linearity and Sensitivity ......................................................................................... 38
3.2.4 Recovery and Precision .......................................................................................... 40
3.2.5 Cross Validation ...................................................................................................... 43
3.2.6 Applicability .............................................................................................................. 45
3.2.7 Discussion ................................................................................................................. 52
CHAPTER 4. DISCUSSION ................................................................................................ 54
CHAPTER 5. CONCLUSIONS ............................................................................................ 56
REFERENCES ....................................................................................................................... 57

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