The evaluation of catechins reducing heterocyclic aromatic amine formation: Structure-activity relationship and mechanism speculation.

The favorable inhibitory effect of tea polyphenols on heterocyclic aromatic amines (HAAs) has been confirmed in many past studies. The objective of this study was to investigate the structure-activity relationship of catechins that act as inhibitors of HAA formation in chemical models. Two kinds of quantitative structure-activity relationship models for catechin-inhibiting-HAA were established. We chose two kinds of HAAs including 2-amino-1-methyl-6-phenylimidazo[4,5-b]pyridine (PhIP) and 2-amino-3,8-dimethylimidazo[4,5-f]quinoxaline (MeIQx), and five catechins including epigallocatechin gallate (EGCG), epicatechin gallate (ECG), epigallocatechin (EGC), epicatechin (EC), and catechin (C). The inhibitory effect of five catechins were in the following order: EGCG > ECG > EGC > C > EC. Thereinto, EGCG and ECG showed dramatically better inhibition on the formation of PhIP and MeIQx, especially EGCG. Further, the mechanisms of catechin-inhibiting-HAA were speculated by correlation analysis. The free radical-scavenging ability was predicted to be the most relevant to the inhibitory effect of ECG, EGC, EC and C on HAAs. Differently, the phenylacetaldehyde-trapping ability might be the more important mechanism of EGCG inhibiting PhIP in chemical model system. This study may bring a broader idea for controlling the formation of HAAs according to the structure of catechins.

A systematic study on the chemical model of polycyclic aromatic hydrocarbons formation from nutrients (glucose, amino acids, fatty acids) in food.

Polycyclic aromatic hydrocarbons (PAHs), prominent carcinogens formed during food processing, pose health risks through long-term consumption. This study focuses on 16 priority PAHs in the European Union, investigating their formation during pyrolysis. Glucose, amino acids and fatty acids are important food nutrients. To further explore whether these nutrients in food form PAHs during heating, a single chemical model method was used to heat these nutrients respectively, and GC-MS/MS was used to identify and quantify the obtained components. Glucose is the most basic nutrient in food, so the influence of water, pH, temperature and other factors on the formation of PAHs was studied in the glucose model. At the same time, the models of amino acids and fatty acids were used to assist in improving the entire nutrient research system. According to our results, some previously reported mechanisms of PAHs formation by fatty acids heating were confirmed. In addition, glucose and amino acids could also produce many PAHs after heating, and some conclusions were improved by comparing the intermediates of PAHs from three types of nutrients.

Exploring the roles of excess amino acids, creatine, creatinine, and glucose in the formation of heterocyclic aromatic amines by UPLC-MS/MS.

The prevention and control of heterocyclic aromatic amines (HAA) formation to mitigate of potential risks to humans, can be achieved by targeting their precursors. In this study, the detailed roles of individual and excess component (20 common α-amino acids, creatine, creatinine, and glucose) on HAA formation in roasted beef patties were examined using UPLC-MS/MS. The results confirmed the reported classical precursors of HAAs. Some components regulated the competitive production of Norharman and Harman. Glycine (Gly) and glucose favored Norharman formation, while cysteine (Cys) and phenylalanine (Phe) for Harman. Serine (Ser) and threonine (Thr) were identified as potential precursors for IQx-type HAAs. Interestingly, methionine (Met), Gly, Thr, Cys, alanine (Ala), and Ser were revealed as more targeted underlying precursors for 1,6-DMIP and 1,5,6-TMIP, and the formation mechanism was inferred. Furthermore, Pro, Leu, His, Ile, Lys and Asp were considered as great inhibitors for HAAs.

A comparative study on inhibition of lung cancer cells by nanoemulsion, nanoliposome, nanogold and their folic acid conjugates prepared with collagen peptides from Taiwan tilapia skin.

Valorization of fish processing waste to obtain value-added products such as collagen and bioactive peptides is a vital strategy to increase the economic value, reduce disposal problems, and prevent harmful impacts on both environment and health. This study aims to isolate two collagen peptides from Taiwan Tilapia skin and prepare 12 nanopeptides including nanoemulsion (NE), nanoliposome (NL), and nanogold (NG) without and with folic acid/chitosan (FA/CH) or FA ligand conjugation for comparison of their inhibition efficiency towards lung cancer cells A549 and normal lung cells MRC5. Acid-soluble collagen (yield, 21.58 %) was extracted using 0.5 M acetic acid and hydrolyzed to obtain two tilapia skin collagen peptides TSCP1 (482 Da) and TSCP2 (172 Da) respectively using 2.5 % and 12.5 % alcalase, with sample-to-water ratio at 1:30 (w/v), pH 8, temperature 50 °C, and hydrolysis time 6 h. Characterization of collagen peptides revealed the presence of type 1 collagen with a high amount of amino acids including glycine (32.6-33.1 %), alanine (13.6-14.0 %), proline (10.0-10.5 %), and hydroxyproline (7.3-7.6 %). TSCP1, TSCP2, and 12 nanopeptides showed a higher cytotoxicity towards A549 cells than MRC5 cells, with TSCP2 and its 6 nanopeptides exhibiting a lower IC50 compared to TSCP1 and its 6 nanopeptides. The mean particle size was 15.7, 33.6, and 16.0 nm respectively for TSCP2-NE, TSCP2-NL, and TSCP2-NG, but changed to 14.4, 36.3, and 17.9 nm following ligand conjugation with a shift in zeta potential from negative to positive for TSCP2-NE-FA/CH and TSCP2-NL-FA/CH. All nanopeptides were more effective than peptides in inhibiting the growth of A549 cells, with the lowest IC50 value being shown for TSCP2-NL-FA/CH (5.32 µg/mL), followed by TSCP2-NE-FA/CH (8.3 µg/mL), TSCP2-NE (22.4 µg/mL), TSCP2-NL (82.7 µg/mL), TSCP2-NG-FA (159.8 µg/mL), TSCP2-NG (234.0 µg/mL) and TSCP2 (359.7 µg/mL). Cell proportions of sub-G1, S, and G2/M phases increased dose-dependently, with a possible cell cycle arrest at G2/M phase. The proportion of necrotic cells was the highest for TSCP2, TSCP2-NE, TSCP2-NE-FA/CH, and TSCP2-NL, while that of late apoptotic cells dominated for TSCP2-NL-FA/CH, TSCP2-NG, and TSCP2-NG-FA. Similarly, TSCP2 and its 6 nanopeptides showed a dose-dependent rise in caspase-3, caspase-8, and caspase-9 activities for execution of apoptosis, with the ligand-conjugated nanopeptides being the most efficient, followed by nanopeptides and peptides. The outcome of this study demonstrated an effective strategy for valorization of Taiwan tilapia skin to obtain collagen peptides and their nanopeptides possessing anticancer activity and form a basis for in vivo study in the future.

Analysis of Polycyclic Aromatic Hydrocarbons via GC-MS/MS and Heterocyclic Amines via UPLC-MS/MS in Crispy Pork Spareribs for Studying Their Formation during Frying.

This study aims to explore the effects of frying conditions on the formation of HAs and PAHs in crispy pork spareribs, a popular meat commodity sold on Taiwan's market. Raw pork spareribs were marinated, coated with sweet potato powder, and fried in soybean oil and palm oil at 190 °C/6 min or 150 °C/12 min, followed by an analysis of HAs and PAHs via QuEChERS coupled with UPLC-MS/MS and GC-MS/MS, respectively. Both HAs and PAHs in pork spareribs during frying followed a temperature- and time-dependent rise. A total of 7 HAs (20.34-25.97 µg/kg) and 12 PAHs (67.69-85.10 µg/kg) were detected in pork spareribs fried in soybean oil and palm oil at 150 °C/12 min or 190 °C/6 min, with palm oil producing a higher level of total HAs and a lower level of total PAHs than soybean oil. The content changes of amino acid, reducing sugar, and creatinine played a vital role in affecting HA formation, while the degree of oil unsaturation and the contents of precursors including benzaldehyde, 2-cyclohexene-1-one, and trans,trans-2,4-decadienal showed a crucial role in affecting PAH formation. The principal component analysis revealed that HAs and PAHs were formed by different mechanisms, with the latter being more liable to formation in pork spareribs during frying, while the two-factorial analysis indicated that the interaction between oil type and frying condition was insignificant for HAs and PAHs generated in crispy pork spareribs. Both CcdP (22.67-32.78 µg/kg) and Pyr (16.70-22.36 µg/kg) dominated in PAH formation, while Harman (14.46-17.91 µg/kg) and Norharman (3.41-4.55 µg/kg) dominated in HA formation in crispy pork spareribs during frying. The outcome of this study forms a basis for learning both the variety and content of HAs and PAHs generated during the frying of pork spareribs and the optimum frying condition to minimize their formation.

Correction: Huang, Y.-C.; Chen, B.-H. A Comparative Study on Improving Streptozotocin-Induced Type 2 Diabetes in Rats by Hydrosol, Extract and Nanoemulsion Prepared from Cinnamon Leaves. Antioxidants 2023, 12, 29.

In the original publication [...].

Effects of Oil and Processing Conditions on Formation of Heterocyclic Amines and Polycyclic Aromatic Hydrocarbons in Pork Fiber.

Toxic compounds such as heterocyclic amines (HAs) and polycyclic aromatic hydrocarbons (PAHs) can be produced during food processing, especially meat products. This study aims to monitor the formation of HAs and PAHs in fried pork fiber, a common meat product in Taiwan, at different processing conditions. A total of six experimental groups, including raw pork tenderloin, dried pork filaments, sesame oil-stir-fried pork at 160 °C for 15 min, sesame oil-stir-fried pork at 200 °C for 6 min, lard-stir-fried pork at 160 °C for 15 min, and lard-stir-fried pork at 200 °C for 6 min, were prepared and analyzed for formation of HAs via UPLC-MS/MS and PAHs via GC-MS/MS in triplicate. Frying in sesame oil or lard showed a greater content of total HAs in fried pork fiber processed at 160 °C for 15 min than at 200 °C for 6 min. However, in the same heating conditions, pork fiber fried in sesame oil produced a higher level of total HAs than that fried in lard. Of the various HAs in fried pork fiber, both Harman and Norharman were generated in the highest amount. The precursors, including reducing sugar, amino acid, and creatine/creatinine, played a vital role in HAs formation in fried pork fiber. For total PAHs, the highest level was shown for pork fiber fried in lard at 200 °C/6 min, followed by frying in sesame oil at 200 °C/6 min and 160 °C/15 min, and in lard at 160 °C/15 min. Like HAs, at the same heating condition, a greater content of total PAHs was produced in pork fiber fried in sesame oil than in lard. Notably, the highly toxic benzo[a]pyrene was undetected in fried pork fiber. The PAH precursor benzaldehyde was shown to generate at a much higher level than 2-cyclohexene-1-one and trans,trans-2,4-decadienal in fried pork fiber, and it should play a more important role in PAH formation. Principal component analysis (PCA) also revealed that the formation mechanism of HAs and PAHs in fried pork fiber was different.

Preparation of Nanoemulsions with Low-Molecular-Weight Collagen Peptides from Sturgeon Fish Skin and Evaluation of Anti-Diabetic and Wound-Healing Effects in Mice.

This study aims to isolate collagen peptides from waste sturgeon fish skin, and prepare nanoemulsions for studying their anti-diabetic and wound-healing effects in mice. Collagen peptides were extracted and purified by acetic acid with sonication, followed by two-stage hydrolysis with 0.1% pepsin and 5% flavourzyme, and ultrafiltration with 500 Da molecular weight (MW) cut-off dialysis membrane. Animal experiments were performed with collagen peptides obtained by pepsin hydrolysis (37 kDa) and pepsin plus flavourzyme hydrolysis (728 Da) as well as their nanoemulsions prepared at two different doses (100 and 300 mg/kg/day). The mean particle size of low-MW and low-dose nanoemulsion, low-MW and high-dose nanoemulsion, high-MW and low-dose nanoemulsion and high-MW and high-dose nanoemulsion was, respectively, 16.9, 15.3, 28.1 and 24.2 nm, the polydispersity index was 0.198, 0.215, 0.231 and 0.222 and zeta potential was -61.2, -63.0, -41.4 and -42.7 mV. These nanoemulsions were highly stable over a 90-day storage period (4 °C and 25 °C) and heating at 40-100 °C (0.5-2 h). Experiments in mice revealed that the low-MW and high-dose nanoemulsion was the most effective in decreasing fasting blood glucose (46.75%) and increasing wound-healing area (95.53%). Collectively, the sturgeon fish skin collagen peptide-based nanoemulsion is promising for development into a health food or wound-healing drug.

Analysis of bioactive compounds in cinnamon leaves and preparation of nanoemulsion and byproducts for improving Parkinson's disease in rats.

Introduction: Cinnamomum osmophloeum Kanehira (C. osmophloeum), a broad-leaved tree species of Taiwan, contains phenolic acids, flavonoids, and phenylpropanoids such as cinnamaldehyde and cinnamic acid in leaves. Many reports have shown that the cinnamon leaf extract possesses anti-inflammatory, hypoglycemic, hypolipidemic and neuroprotective functions. This study aims to analyze bioactive compounds in C. osmophloeum (cinnamon leaves) by UPLC-MS/MS and prepare hydrosol, cinnamon leaf extract and cinnamon leaf nanoemulsion for comparison in improving Parkinson's disease (PD) in rats. Methods: After extraction and determination of total phenolic and total flavonoid contents, cinnamaldehyde and the other bioactive compounds were analyzed in cinnamon leaves and hydrosol by UPLC-MS/MS. Cinnamon leaf nanoemulsion was prepared by mixing a suitable proportion of cinnamon leaf extract, soybean oil, lecithin, Tween 80 and deionized water, followed by characterization of particle size and polydispersity index by dynamic light scattering analyzer, particle size and shape by transmission electron microscope, encapsulation efficiency, as well as storage and heating stability. Fifty-six male Sprague-Dawley rats aged 8 weeks were divided into seven groups with group 1 as control (sunflower oil) and group 2 as induction (2 mg/kg bw rotenone in sunflower oil plus 10 mL/kg bw saline), while the other groups including rotenone injection (2 mg/kg bw) followed by high-dose of 60 mg/kg bw (group 3) or low-dose of 20 mg/kg bw (group 4) for tube feeding of cinnamon leaf extract or cinnamon leaf nanoemulsion at the same doses (groups 5 and 6) every day for 5 weeks as well as group 7 with rotenone plus hydrosol containing 0.5 g cinnamon leaf powder at a dose of 10 mL/kg bw. Biochemical analysis of brain tissue (striatum and midbrain) was done to determine dopamine, α-synuclein, tyrosine hydroxylase, superoxide dismutase, catalase, glutathione peroxidase and malondialdehyde contents by using commercial kits, while catalepsy performed by bar test. Results and discussion: An extraction solvent of 80% ethanol was found to be the most optimal with a high yield of 15 bioactive compounds being obtained following UPLC analysis. A triple quadrupole tandem mass spectrometer with electrospray ionization mode was used for identification and quantitation, with cinnamaldehyde present at the highest amount (17985.2 µg/g). The cinnamon leaf nanoemulsion was successfully prepared with the mean particle size, zeta potential, polydispersity index and encapsulation efficiency being 30.1 nm, -43.1 mV, 0.149 and 91.6%, respectively. A high stability of cinnamon leaf nanoemulsion was shown over a 90-day storage period at 4 and heating at 100 for 2 h. Animal experiments revealed that the treatments of cinnamon leaf extract, nanoemulsion and hydrosol increased the dopamine contents from 17.08% to 49.39% and tyrosine hydroxylase levels from 17.07% to 25.59%, while reduced the α-synuclein levels from 17.56% to 15.95% in the striatum of rats. Additionally, in the midbrain of rats, an elevation of activities of superoxide dismutase (6.69-16.82%), catalase (8.56-16.94%), and glutathione peroxidase (2.09-16.94%) was shown, while the malondialdehyde content declined by 15.47-22.47%. Comparatively, the high-dose nanoemulsion exerted the most pronounced effect in improving PD in rats and may be a promising candidate for the development of health food or botanic drug.

Analysis of Phenolic Acids and Flavonoids in Rabbiteye Blueberry Leaves by UPLC-MS/MS and Preparation of Nanoemulsions and Extracts for Improving Antiaging Effects in Mice.

Rabbiteye blueberry leaves, a waste produced after harvest of blueberry, are rich in polyphenols. This study aims to analyze phenolic acids and flavonoids in blueberry leaves by UPLC-MS/MS and prepare nanoemulsions for determining anti-aging activity in mice. Overall, 30% ethanol was the most suitable extraction solvent for total phenolic acids and total flavonoids. A total of four phenolic acids and four flavonoids were separated within seven minutes for further identification and quantitation by UPLC-MS/MS in selective reaction monitoring (SRM) mode, with 3-O-caffeoylquinic acid being present in the highest amount (6474.2 µg/g), followed by quercetin-3-O-galactoside (1943.9 µg/g), quercetin-3-O-rutinoside (1036.6 µg/g), quercetin-3-O-glucoside (867.2 µg/g), 5-O-caffeoylquinic acid (815.8 µg/g), kaempferol-3-O-glucoside (309.7 µg/g), 3,5-dicaffeoylquinic acid (195.3 µg/g), and 4,5-dicaffeoylquinic acid (60.8 µg/g). The blueberry nanoemulsion was prepared by using an appropriate ratio of soybean oil, Tween 80, glycerol, ethanol, and water at 1.2%, 8%, 2%, 2%, and 86.8%, respectively, and mixing with dried blueberry extract, with the mean particle size and zeta potential being 16 nm and -54 mV, respectively. A high stability was observed during storage of nanoemulsion for 90 days at 4 °C and heated at 100 °C for 2 h. An animal study revealed that this nanoemulsion could elevate dopamine content in mice brain as well as superoxide dismutase, glutathione peroxidase, and catalase activities in mice liver while reducing the contents of malondialdehyde and protein carbonyl in mice brains. Collectively, the high-dose nanoemulsion possessed the highest efficiency in improving mice aging with a promising potential for development into a health food.

Analysis of Furan and Its Derivatives in Food Matrices Using Solid Phase Extraction Coupled with Gas Chromatography-Tandem Mass Spectrometry.

The objective of this study was to develop a simultaneous analysis method of furan and its 10 derivatives in different food commodities. The results indicated that furan and its 10 derivatives could be separated within 9.5 min by using a HP-5MS column and gas chromatography-tandem mass spectrometry (GC-MS/MS) with multiple reaction monitoring mode for detection. Furthermore, this method could resolve several furan isomers, such as 2-methyl furan and 3-methyl furan, as well as 2,3-dimethyl furan and 2,5-dimethyl furan. The most optimal extraction conditions were: 5 g of the fruit or juice sample mixed with 5 mL of the saturated NaCl solution, separately, or 1 g of the canned oily fish sample mixed with 9 mL of the saturated NaCl solution, followed by the equilibration of each sample at 35 °C for 15 min, using a carboxen-polydimethylsiloxane SPME arrow to adsorb the analytes for 15 min at 35 °C for subsequent analysis by GC-MS/MS. For method validation of all the analytes in the different food matrices, the recovery was 76-117% and the limit of the quantitation was 0.003-0.675 ng/g, while the relative standard deviation (RSD%) of the intra-day variability range from 1-16%, and that of the inter-day variability was from 4-20%. The method validation data further demonstrated that a reliable method was established for the analysis of furan and its 10 derivatives in commercial foods.

Quantification of Xanthone and Anthocyanin in Mangosteen Peel by UPLC-MS/MS and Preparation of Nanoemulsions for Studying Their Inhibition Effects on Liver Cancer Cells.

Mangosteen peel, a waste produced during mangosteen processing, has been reported to be rich in xanthone and anthocyanin, both of which possess vital biological activities such as anti-cancer properties. The objectives of this study were to analyze various xanthones and anthocyanins in mangosteen peel by UPLC-MS/MS for the subsequent preparation of both xanthone and anthocyanin nanoemulsions to study their inhibition effects on liver cancer cells HepG2. Results showed that methanol was the optimal solvent for the extraction of xanthones and anthocyanins, with a total amount of 68,543.39 and 2909.57 µg/g, respectively. A total of seven xanthones, including garcinone C (513.06 µg/g), garcinone D (469.82 µg/g), γ-mangostin (11,100.72 µg/g), 8-desoxygartanin (1490.61 µg/g), gartanin (2398.96 µg/g), α-mangostin (51,062.21 µg/g) and ß-mangostin (1508.01 µg/g), as well as two anthocyanins including cyanidin-3-sophoroside (2889.95 µg/g) and cyanidin-3-glucoside (19.72 µg/g), were present in mangosteen peel. The xanthone nanoemulsion was prepared by mixing an appropriate portion of soybean oil, CITREM, Tween 80 and deionized water, while the anthocyanin nanoemulsion composed of soybean oil, ethanol, PEG400, lecithin, Tween 80, glycerol and deionized water was prepared as well. The mean particle size of the xanthone extract and nanoemulsion were, respectively, 22.1 and 14.0 nm as determined by DLS, while the zeta potential was -87.7 and -61.5 mV. Comparatively, xanthone nanoemulsion was more effective than xanthone extract in inhibiting the growth of HepG2 cells, with the IC50 being 5.78 µg/mL for the former and 6.23 µg/mL for the latter. However, the anthocyanin nanoemulsion failed to inhibit growth of HepG2 cells. Cell cycle analysis revealed that the proportion of the sub-G1 phase followed a dose-dependent increase, while that of the G0/G1 phase showed a dose-dependent decline for both xanthone extracts and nanoemulsions, with the cell cycle being possibly arrested at the S phase. The proportion of late apoptosis cells also followed a dose-dependent rise for both xanthone extracts and nanoemulsions, with the latter resulting in a much higher proportion at the same dose. Similarly, the activities of caspase-3, caspase-8 and caspase-9 followed a dose-dependent increase for both xanthone extracts and nanoemulsions, with the latter exhibiting a higher activity at the same dose. Collectively, xanthone nanoemulsion was more effective than xanthone extract in inhibiting the growth of HepG2 cells. Further research is needed to study the anti-tumor effect in vivo.

Formation and Inhibition of Heterocyclic Amines and Polycyclic Aromatic Hydrocarbons in Ground Pork during Marinating.

This study aims to simultaneously extract heterocyclic amines (HAs) and polycyclic aromatic hydrocarbons (PAHs) from ground pork for respective analysis by UPLC-MS/MS and GC-MS/MS, and study the effects of different flavorings and marinating time length on their formation and inhibition. Results showed that both HA and PAH contents followed a time-dependent increase during marinating, with HAs being more susceptible to formation than PAHs. The total HA contents in unmarinated pork and juice was, respectively, 61.58 and 139.26 ng/g, and rose to 2986.46 and 1792.07 ng/g after 24-h marinating, which can be attributed to the elevation of reducing sugar and creatinine contents. The total PAH contents in unmarinated pork and juice were, respectively, 34.56 and 26.84 ng/g, and increased to 55.93 and 44.16 ng/g after 24-h marinating, which can be due to the increment of PAH precursors such as benzaldehyde, 2-cyclohexene-1-one and trans,trans-2,4-decadienal. Incorporation of 0.5% (w/v) cinnamon powder or 0.5% (w/v) green tea powder was effective in inhibiting HA formation with the former showing a more pronounced effect for marinated pork, while the latter was for marinated juice. However, their addition was only effective in inhibiting PAH formation in marinated pork. Principle component analysis revealed the relationship between HA and PAH formation in ground pork and juice during marinating.

Development of a GC-MS/MS method coupled with HS-SPME-Arrow for studying formation of furan and 10 derivatives in model systems and commercial foods.

Furan has been described as a carcinogen, being present in numerous food products available to the everyday consumer. The objectives of this study were to determine the formation of furan and its derivatives in 3 model systems during heating, with their contents being determined in selected commercial food products by HS-SPME Arrow coupled with GC/MS/MS. A high accuracy and precision was attained for the method developed in this study. The model system of 0.5 M glucose/alanine + 0.1 M ascorbic acid generated the highest furan level (5603.63 ng/g) when heated at 121 °C for 2 h. The addition of ascorbic acid favored formation of furfural and furfuryl alcohol, while linoleic acid favored formation of furfuryl alcohol. In addition, the total furan contents in various commercial foods ranged from 21.14 to 3183.39 ng/g. Most importantly, the outcome of model systems may be used to predict the presence of furan and its derivatives in commercial foods.

Improved Analytical Method for Determination of Furan and Its Derivatives in Commercial Foods by HS-SPME Arrow Combined with Gas Chromatography-Tandem Mass Spectrometry.

Owing to the presence of significant levels of toxic furan compounds reported globally in commercial foods by various food authorities, the objectives of this study were to develop an analytical method for determination of furan and its 10 derivatives in commercial foods using headspace-solid phase microextraction (HS-SPME)-Arrow coupled with gas chromatography-tandem mass spectrometry. Furan and its 10 derivatives were separated within 10 min by employing an HP-5MS capillary column with d4-furan as the internal standard for quantitation. The most optimal sample weight and extraction time for various commercial food samples, respectively, ranged from 1 to 5 g and 10-15 min depending on the sample variety. For extraction, carboxen/poly(dimethylsiloxane) (CAR/PDMS) cellulose was used with the temperature at 30 °C, equilibration time of 15 min, and desorption time of 3 min. The limit of detection ranged from 0.001 to 1.071 ng/g, while the limit of quantitation ranged from 0.003 to 3.571 ng/g. A high precision and accuracy were obtained for this method. The total furan content in commercial foods ranged from nd to 40 725.85 ng/g, in which the mean contents were the highest for brewed coffee (35 082.26 ng/g) and canned coffee (25 152.22 ng/g), while the lowest were for potato chip and cookies (0.57-1.48 ng/g), donut (1.50 ng/g), milk (0.34-30.38 ng/g), and oat (6.56 ng/g).

A Comparative Study on Analysis of Ginsenosides in American Ginseng Root Residue by HPLC-DAD-ESI-MS and UPLC-HRMS-MS/MS.

Ginseng (Panax quinquefolius), a popular herbal and nutritional supplement consumed worldwide, has been demonstrated to possess vital biological activities, which can be attributed to the presence of ginsenosides. However, the presence of ginsenosides in ginseng root residue, a by-product obtained during processing of ginseng beverage, remains unexplored. The objectives of this study were to develop a high-performance liquid chromatography-photodiode array detection-mass spectrometry (HPLC-DAD-ESI-MS) and an ultra-high-performance-liquid-chromatography-tandem mass spectrometry (UPLC-HRMS-MS/MS) method for the comparison of ginsenoside analysis in ginseng root residue. Results showed that by employing a Supelco Ascentis Express C18 column (150 × 4.6 mm ID, particle size 2.7 µm) and a gradient mobile phase of deionized water and acetonitrile with a flow rate at 1 mL/min and detection at 205 nm, a total of 10 ginsenosides, including internal standard saikosaponin A, were separated within 18 min and detected by HPLC-DAD-ESI-MS. Whereas with UPLC-HRMS-MS/MS, all the 10 ginsenosides were separated within six minutes by using an Acquity UPLC BEH C18 column (50 × 2.1 mm ID, particle size 1.7 µm, 130 Å) and a gradient mobile phase of ammonium acetate and acetonitrile with column temperature at 50 °C, flow rate at 0.4 mL/min and detection by selected reaction monitoring (SRM) mode. High accuracy and precision was shown, with limit of quantitation (LOQ) ranging from 0.2−1.9 µg/g for HPLC-DAD-ESI-MS and 0.269−6.640 ng/g for UPLC-HRMS-MS/MS. The contents of nine ginsenosides in the ginseng root residue ranged from

A Comparative Study on Inhibition of Breast Cancer Cells and Tumors in Mice by Carotenoid Extract and Nanoemulsion Prepared from Sweet Potato (Ipomoea batatas L.) Peel.

The objectives of this study were to determine carotenoid composition in sweet potato (TNG66) peel and prepare carotenoid nanoemulsion to study its inhibition effect on breast cancer cells MCF-7 and tumors in mice. Results showed that a total of 10 carotenoids were separated within 30 min by employing a YMC C30 column and a gradient mobile phase of methanol/acetonitrile/water (74:14:12, v/v/v) and dichloromethane (B) with a flow rate of 1 mL/min, column temperature of 25 °C, and detection wavelength of 450 nm. Following quantitation, all-trans-ß-carotene was present in the highest amount (663.8 µg/g). The method validation data demonstrated a high accuracy and precision of this method. The carotenoid nanoemulsion was prepared by mixing an appropriate proportion of carotenoid extract, Tween 80, PEG 400, soybean oil and deionized water with the mean particle size being 15.7 nm (transmission electron microscope (TEM)), polydispersity index 0.238, encapsulation efficiency 97% and zeta potential -69.8 mV. A high stability of carotenoid nanoemulsion was shown over a 90-day storage period at 25 °C and during heating at 100 °C for 2 h. The release percentage of total carotenoids from carotenoid nanoemulsion under gastric and intestinal condition was 18.3% and 49.1%, respectively. An antiproliferation study revealed that carotenoid nanoemulsion was more effective than carotenoid extract in inhibiting the growth of human breast cancer cells MCF-7. Following treatments of paclitaxel (10 µg/mL), carotenoid nanoemulsion (20 and 10 µg/mL) and carotenoid extract (20 and 10 µg/mL), the tumor weight of mice respectively decreased by 77.4, 56.2, 40.3, 36.1 and 18.7%, as well as tumor volume of mice by 75.4, 65.0, 49.7, 46.7 and 26.5%. Also, both carotenoid extract and nanoemulsion could reduce the levels of epidermal growth factor (EGF) and (vascular endothelial growth factor (VEGF) in serum, with the latter being more effective. This finding suggested that carotenoid nanoemulsion was more effective than carotenoid extract in inhibiting tumor growth in mice.

An improved surface enhanced Raman spectroscopic method using a paper-based grape skin-gold nanoparticles/graphene oxide substrate for detection of rhodamine 6G in water and food.

Organic toxins are persistent chemicals of global concern capable of accumulating in environment and food. Surface enhanced Raman spectroscopy (SERS) is a promising technique that facilitates onsite detection of organic toxins. However, the fabrication of a SERS substrate is complicated and difficult to provide flexibility, fastness and cost-effectiveness. This study aims to develop a paper-based SERS method using grape skin-gold nanoparticles/graphene oxide (GE-AuNPs/GO) as SERS substrate and evaluate its efficiency with rhodamine 6G (Rh6G) as a model organic toxin and a real water and food contaminant. GE-AuNPs synthesized by green method using grape skin waste extract and GE-AuNPs/GO showed a surface plasmon resonance at 536 and 539 nm, particle size 18.6 and 19.5 nm, and zeta potential -44.6 and -59.7 mV, respectively. Paper-based SERS substrates were prepared by coating a hydrophobic thin-film of 30% polydimethylsiloxane solution in hexane on Whatman no. 1 filter paper, followed by drop-casting GE-AuNPs or GE-AuNPs/GO and drying. The SERS signals of Rh6G showed an enhancement factor of 5.8 × 104 for GE-AuNPs and 1.92 × 109 for GE-AuNPs/GO, implying that a combination of electromagnetic surface plasmon, charge transfer and molecular resonances may be responsible for a higher enhancement of signal by the latter. A low detection limit of 7.33 × 10-11 M in the linear range of 10-11-10-5 M was obtained for GE-AuNPs/GO, while the relative standard deviation of repeatability and reproducibility was 9.6 and 12.6%, respectively. Paper-based GE-AuNPs/GO SERS substrate was highly stable as <20% loss in efficiency was shown over a 60-day storage period. Application to real samples showed a high recovery of Rh6G from tap water (93.9-100.8%) as well as food samples such as red chilli powder (91.0-95.4%), red glutinous rice ball (96.6-98.3%) and tomato ketchup (98.9-102.3%) after QuEChERS extraction. Collectively, the developed paper-based GE-AuNPs/GO can be a potential substrate for sensitive onsite detection of rhodamine 6G by SERS method.

A Comparative Study on Improving Streptozotocin-Induced Type 2 Diabetes in Rats by Hydrosol, Extract and Nanoemulsion Prepared from Cinnamon Leaves.

Cinnamomoum osmophloeum Kanehira (C. osmophloeum) contains various biologically active antioxidant compounds such as flavonoids, phenolic acids and cinnamaldehyde. Type 2 diabetes mellitus is a chronic disease of metabolic abnormality caused by insulin deficiency or resistance. The objectives of this study were to analyze various bioactive compounds in C. osmophloeum leaves by ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), and compare the effects of hydrosol, extract and nanoemulsion prepared from C. osmophloeum leaves on improving type 2 diabetes in rats. Our results show that a total of 15 bioactive compounds in C. osmophloeum leaves, including quercetin, quercetin-3-O-galactoside, quercetin-3-O-glucoside, rutin, caffeic acid, benzoic acid, 5-O-caffeoylquinic acid, kaempferol 3-ß-D-glucopyranoside, trans-cinnamic acid, coumarin, cinnamyl alcohol, p-coumaric acid, eugenol, kaempferol and cinnamaldehyde, were separated within 14 min for subsequent identification and quantitation by UPLC-MS/MS. The nanoemulsion was successfully prepared by mixing C. osmophloeum leaf extract, soybean oil, lecithin, Tween 80 and deionized water in an appropriate proportion with a mean particle size, polydispersity index, zeta potential and encapsulation efficiency of 36.58 nm, 0.222, -42.6 mV and 91.22%, respectively, while a high storage and heating stability was obtained. The animal experiment results reveal that the high-dose nanoemulsion was the most effective in reducing both fasting blood glucose and oral glucose tolerance test value, followed by low-dose nanoemulsion, high-dose extract, low-dose extract and leaf powder in hydrosol. A similar trend was shown in reducing serum insulin and the homeostatic model assessment of insulin resistance index. In addition, the contents of serum biochemical parameters, including total cholesterol, triglyceride, aspartate aminotransferase, alanine aminotransferase, uric acid, urea nitrogen and creatinine, were reduced, with the high-dose nanoemulsion showing the most pronounced effect. Collectively, the high-dose nanoemulsion may possess great potential to be developed into a hypoglycemic health food or botanic drug.