The effects of 9 different solvents on the measurement of the total phenolics and antioxidant activities of mulberry fruits were studied using accelerated solvent extraction (ASE). Sixteen to 22 types of phenolics (flavonols, flavan-3-ols, flavanol, hydroxycinnamic acids, hydroxybenzoic acids, and stilbenes) from different mulberry extracts were characterized and quantified using HPLC-MS/MS. The principal component analysis (PCA) was used to determine the suitable solvents to distinguish between different classes of phenolics. Additionally, the phenolic extraction abilities of ASE and ultrasound-assisted extraction (UAE) were compared. The highest extraction efficiency could be achieved by using 50% acidified methanol (50MA) as ASE solvents with 15.14 mg/gallic acid equivalents g dry weight of mulberry fruit. The PCA results revealed that the 50MA followed by 50% acidified acetone (50AA) was the most efficient solvent for the extraction of phenolics, particularly flavonols (627.12 and 510.31 μg/g dry weight, respectively), while water (W) was not beneficial to the extraction of all categories of phenolics. Besides, the results of 3 antioxidant capability assays (DPPH, ABTS free radical-scavenging assay, and ferric-reducing antioxidant power assay) showed that water-based organic solvents increased the antioxidant capabilities of the extracts compared with water or pure organic solvents. ASE was more suitable for the extraction of phenolics than UAE.
A total of 56 dried vine fruits, including 31 sultanas and 25 currants, were selected from Chinese markets in 2012. All samples were analysed for Ochratoxin A (OTA) using solid-phase extraction and high-performance liquid chromatography (HPLC) with fluorescence detection. It turned out that 58.9% of the samples were positive and the OTA amount ranged from <0.07 to 12.83 μg/kg, with a mean level of 0.99 μg/kg. Only one sample exceeded the European Union (EU) maximum level of 10 μg/kg. Meanwhile, it was shown that OTA contamination increased among north-western, northern and southern China, which showed OTA means of 0.08, 0.99 and 2.01 μg/kg, respectively. Moreover, in samples of products sold in sealed plastic bags, i.e. consumer-size packages (n = 19, mean = 0.30 μg/kg) less OTA was detected when compared with sampled bulk packages (n = 37, mean = 1.67 μg/kg). In addition, sultanas (mean = 0.92 μg/kg) had less OTA contamination than currants (mean = 1.22 μg/kg).
In China, peanut sprouts are popular among consumers as functional vegetables. This study reports the change in total phenolic content (TPC), total flavonoid content (TFC), monomeric anthocyanin content (MAC), vitamin C, trans-resveratrol content, antioxidant capacities, and phenolic profile of three different varieties of peanut during 8 days of germination. The TPC, TFC, and antioxidant capacity of peanut samples were reduced and then increased with an increase in germination time. TFC values were highly correlated with 2,2-diphenyl-1-picrylhydrazyl (DPPH) and ferric reducing antioxidant power (FRAP) values. MAC values of peanuts were first increased and then decreased during 8 days of germination. The TFC, DPPH, and FRAP values of germinated peanuts were lower compared to the non-germinated peanut. Germination of peanut samples enhanced the total phenolic acids and trans-resveratrol content, but the vitamin C content of peanut sprouts was lower than ungerminated peanuts.
A simple, sensitive and reliable quantification and identification method was developed for simultaneous analysis of ochratoxin A (OTA) and its related metabolites ochratoxin alpha (OTα), ochratoxin B (OTB) and mellein. The method was assessed by spiking analytes into blank culture media and dried vine fruits. Performance was tested in terms of accuracy, selectivity and repeatability. The method involves an ultrasonic extraction step for culture samples using methanol aqueous solution (7:3, v/v); the mycotoxin is quantified by high-performance liquid chromatography coupled with electrospray ionisation and triple quadrupole mass spectrometry (LC-ESI-MS/MS). The recoveries were 74.5-108.8%, with relative standard deviations (RSDs) of 0.4-8.4% for fungal culture. The limits of detection (LODs) were in the range of 0.03-0.87 μg l(-)(1), and the limits of quantification (LOQs) ranged from 0.07 to 2.90 μg l(-)(1). In addition, the extraction solutions and clean-up columns were optimised specifically for dried vine fruit samples to improve the performance of the method. Methanol-1% sodium bicarbonate extraction solution (6:4, v/v) was determined to be the most efficient. Solid-phase extraction (SPE) was performed as a clean-up step prior to HPLC-MS/MS analysis to reduce matrix effects. Recoveries ranged from 80.1% to 110.8%. RSDs ranged from 0.1% to 3.6%. LODs and LOQs ranged from 0.06 to 0.40 μg kg(-)(1) and from 0.19 to 1.20 μg kg(-)(1), respectively. The analytical method was established and used to identify and quantify OTA and related compounds from Aspergillus carbonarius and Aspergillus ochraceus in cultures and dried vine fruits. The results showed that A. carbonarius produced OTα, OTB and OTA, whereas A. ochraceus produced OTB, OTA and mellein after 7 days of cultivation. Of 30 commercial samples analysed, 10 were contaminated with ochratoxins; OTB, OTα and mellein were also detected in different samples.
A method was developed for the determination of the mycotoxin ochratoxin A in dried jujube (Zizyphus jujuba Miller) using alkaline methanolic extraction, immunoaffinity column clean-up (IAC) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) determination. The limit of detection (LOD) was 0.01 μg kg(-1) and limit of quantification (LOQ) was 0.03 μg kg(-1). The average recoveries were 82%, 98% and 115% at 5, 0.5 and 0.1 μg kg(-1) spiked levels with relative standard deviations (RSD) of 2.9%, 5.2% and 9.2% accordingly. The method showed good linearity for both solvent standard calibration and matrix-matched standard calibration with correlation coefficients of 0.9998 and 0.9997 respectively. The intra-day precision RSD was 3.3% and the inter-day precision RSD was 4.0%. In addition, there was almost no matrix interference in LC-MS/MS detection after the IAC clean-up process. The proposed analytical set-up was successfully used to test 20 samples that were collected from local markets and stores. The results showed that all the samples were positive and the amount of OTA ranged from < 0.01 to 0.18 μg kg(-1), with a mean level of 0.14 μg kg(-1). In spite of the high positive rate, samples with this level would not cause significant health effects after consumption.
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