流动注射原子吸收光谱法测定富硒天麻、葡萄及大米中的硒

建立了流动注射氢化物发生-原子吸收光谱法测定富硒天麻、葡萄及大米中硒的方法。测定硒的线性范围为0．33μg/L-50μg/L，相对标准偏差小于3％，加标回收率为93％-106％。方法已广泛应用于实际样品中微量硒的测定。     

Influence of the tannin structure on the disruption effect of carbohydrates on protein-tannin aggregates

The disrupting effect of three different ionic carbohydrates (xanthan, pectin and gum arabic) on the formation of tannin-protein insoluble aggregates was assessed by nephelometry using bovine serum albumin (BSA) and several procyanidin fractions previously extracted from grape seeds. The presence in solution of any of the carbohydrates studied was found to restrain the formation of insoluble protein-tannin aggregates for every procyanidin fraction used. Xanthan was the most effective carbohydrate, whereas gum arabic was the least effective. The present work has revealed that the disrupting effect of carbohydrates is quite different depending on the procyanidin structure complexity. In general, the three carbohydrates studied revealed a similar trend in that their disrupting effect on tannin-BSA aggregate formation decreased with increase of the procyanidin degree of polymerization.     

Antioxidant potential in the leaves of grape varieties (Vitis vinifera L.) grown in different soil compositions

Grape plant (Vitis vinifera L.) is a species of the family Vitaceae. It is an economically important fruit plant abundantly grown all over the world. Vitaceae comprised of 900 species distributed across tropical, sub-tropical and partially temperate sorts of climatic zones. In the current study we aimed to evaluate the antioxidant activities of grape leaves extract from different Pakistani varieties.We have analyzed the crude methanolic extract from the leaves of Pakistani grape varieties (i.e. NARC Black, Sundar Khani, Shogran-1, Shogran-2, Haita, Sheghali, Perlette, and Sultania-C) cultivated in various soil compositions. Total phenolic contents (TPC) of the extract were determind by using Folin-ciocalteu reagent method. Total flavonoid contents (TFC) were determind by the Aluminum Chloride Calorimetric method. Antioxidant activities of the extracts of different concentration were evaluated using Phosphomolybdenum method, Reducing power and DPPH (2, 2-disphenyl-1-picryl-hydrazyl) assays. Assays performed for grape varieties showed great antioxidant potential. All varieties significantly depicted with variation in polyphenolic contents and antioxidant potential with changes in the soil conditions. The highest TPC and TFC were quantified in Shogran-1 97.58 ± 0.09 (GAE, g⁻¹) and Sultania-C 97.47 ± 0.12 (µg QE/g DE) varieties respectively which were grown in (T6) and (T5), while lower were recorded in Sundar khani 5.16 ± 0.23 in (T6). Likewise, Shogran-1 128.26 ± 0.23 (µg AAE/g extract) variety grown in (T6) depicted highest total antioxidant capacity, NARC black 182.06 ± 0.24 (µg AAE/g extract) variety grown in (T6) resulted in maximum reducing power while DPPH free radical scavenging potential were determinded in Sultania-C 80.91 ± 0.10 (T4) equivalent µg/g. In the terms of bioassays, the promising results were showed by compost + sand + clay (T4), compost + clay + dung (T5) and sand + clay + dung (T6). Therefore, we conclude that variation in soil composition has a significant contribution in the quantity of phytochemicals and antioxidants expression. Our study further suggest that use of organic fertilizer (Compost) and loamy sort of soil enhance functioning of most of the varieties in terms of important phytochemicals.     

气相色谱-正化学源-质谱联用技术测定葡萄和葡萄酒中多种唑类杀菌剂的残留量

建立了可用于葡萄和葡萄酒中20种唑类杀菌剂残留量的分散型固相萃取-气相色谱-正化学离子源质谱分析方法.葡萄和葡萄酒样品分别用乙腈(含1%冰醋酸)和乙酸乙酯提取,分散型固相萃取法净化,由气相色谱-正化学离子源质谱分时段选择离子监测技术进行测定与确证,外标法定量.20种农药在50～1000 μg/L范围内线性均良好; 所有农药的方法定量限(LOQ)均低于10 μg/kg;在3个添加水平(10, 20和40 μg/kg)下,所有农药的回收率均处于71.2%～102.2%之间, RSD≤10.6%.     

UPLC-MS/MS测定葡萄籽提取物中78种农药残留

建立了超高效液相色谱串联质谱法(UPLC-MS/MS)检测葡萄籽提取物中78种农药残留物的分析方法。样品用乙腈振荡提取,经乙二胺-N-丙基甲硅烷(PSA)和石墨化炭(GCB)固相萃取柱串联净化,乙腈-甲苯(V/V3:1)洗脱,洗脱液浓缩至约0.5 mL后,于45℃下氮气吹干,1.0 mL乙腈定容,UPLC-MS/MS测定,外标法定量。葡萄籽提取物中,78种农药在0.001～0.2μg/mL范围内线性关系均良好;所有农药的方法定量限(LOQ)均低于17.0μg/kg;在5,25,50μg/kg的添加水平下,葡萄籽提取物中78种农药的平均回收率处于72.6%～113.5%之间,相对标准偏差不大于11%。方法适用于葡萄籽提取物中78种农药残留的快速筛查测定。     

Application of Fourier transform infrared spectroscopy and orthogonal projections to latent structures/partial least squares regression for estimation of procyanidins average degree of polymerisation

Fourier transform infrared (FTIR) spectroscopy has being emphasised as a widespread technique in the quick assess of food components. In this work, procyanidins were extracted with methanol and acetone/water from the seeds of white and red grape varieties. A fractionation by graded methanol/chloroform precipitations allowed to obtain 26 samples that were characterised using thiolysis as pre-treatment followed by HPLC-UV and MS detection. The average degree of polymerisation (DPn) of the procyanidins in the samples ranged from 2 to 11 flavan-3-ol residues. FTIR spectroscopy within the wavenumbers region of 1800-700 cm⁻¹ allowed to build a partial least squares (PLS1) regression model with 8 latent variables (LVs) for the estimation of the DPn, giving a RMSECV of 11.7%, with a R² of 0.91 and a RMSEP of 2.58. The application of orthogonal projection to latent structures (O-PLS1) clarifies the interpretation of the regression model vectors. Moreover, the O-PLS procedure has removed 88% of non-correlated variations with the DPn, allowing to relate the increase of the absorbance peaks at 1203 and 1099 cm⁻¹ with the increase of the DPn due to the higher proportion of substitutions in the aromatic ring of the polymerised procyanidin molecules.     

Gas chromatographic-mass spectroscopic identification of volatile oil constituents of Omphalocarpus procesum

Summary The steam volatile oil of the seeds ofOmphalocarpus procerum P. Beauv (Sapotaceae) was investigated by capillary gas chromatography with characterisation by mass spectroscopy. The identification of palmitic acid (8%), indole (2.6%), δ-cadinene (7%), cinnamic alcohol (2.12%), α-humulene (0.38%), γ-muurolene (0.49%) as well as smaller amounts of 25 additional compounds was confirmed by GC-MS. In all about 70 compounds were detected in the volatile oil which also contained a large fraction of oxygenated sesquiterpenes.     

Rapid automated high performance liquid chromatography method for simultaneous determination of amino acids and biogenic amines in wine, fruit and honey

This paper reports a new, simple, rapid and economical method for routine determination of 24 amino acids and biogenic amines in grapes and wine. No sample clean-up is required and total run time including column re-equilibration is less than 40min. Following automated in-loop automated pre-column derivatisation with an o-phthaldialdehyde, N-acetyl-l-cysteine reagent, compounds were separated on a 3mm×25cm C(18) column using a binary mobile phase. The method was validated in the range 0.25-10mg/l; repeatability was less than 3% RSD and the intermediate precision ranged from 2 to 7% RSD. The method was shown to be linear by the 'lack of fit' test and the accuracy was between 97 and 101%. The LLOQ varied between 10μg/l for aspartic and glutamic acids, ethanolamine and GABA, and 100μg/l for tyrosine, phenylalanine, putrescine and cadaverine. The method was applied to grapes, white wine, red wine, honey and three species of physalis fruit. Grapes and physalis fruit were crushed, sieved, centrifuged and diluted 1/20 and 1/100, respectively, for analysis; wines and honeys were simply diluted 10-fold. It was shown using this method that the amino acid content of grapes was strongly correlated with berry volume, moderately correlated with sugar concentration and inversely correlated with total acidity.     

Offline combination of pressurized fluid extraction and electron paramagnetic resonance spectroscopy for antioxidant activity of grape skin extracts assessment

A comprehensive characterization of grape skin methanolic and ethanolic extracts prepared by pressurized fluid extraction (PFE) at various temperatures within 40 to 120 °C from two wine grape varieties, St. Laurent and Alibernet was performed. For the first time, an offline combination of PFE and electron paramagnetic resonance (EPR) spectroscopy together with other experimental methods was employed to assess the effect of extraction conditions on numerous extract characteristics including antioxidant or radical-scavenging ability, HPLC profile of anthocyanins, total phenolic compounds content (TPC), tristimulus color values (CIE Lab), and pH values. The properties of extracts depend on the solvent used, the mass of grape skins as well as on the extraction conditions among which the temperature plays a crucial role. In spite of wide interval of extraction temperatures, all extracts still retain their antioxidant and/or radical-scavenging properties, indicating that the extracts prepared by PFE can serve as potential source of functional food supplements or color enhancers.     

Computer controlled-flow injection potentiometric system based on virtual instrumentation for the monitoring of metal-biosorption processes

A completely automated flow-injection system was developed for the monitoring of biosorption studies of Cu(II) ion on vegetable waste by-products. The system employed flow-through Cu(II)-selective electrodes, of epoxy-resin-CuS/Ag₂S heterogeneous crystalline type, and computer controlled pumps and valves for the flow operation. Computer automation was done through a specially devised virtual instrument, which commanded and periodically calibrated the system, allowing for the monitoring of Cu(II) ions between 0.6 and 6530 mg L⁻¹ at a typical frequency of 15 h⁻¹. Grape stalk wastes were used as biosorbent to remove Cu(II) ions in a fixed-bed column with a sorption capacity of 5.46 mg g⁻¹, obtained by the developed flow system, while the reference determination performed by FAAS technique supplied a comparable value of 5.41 mg g⁻¹.