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1.
Annatto is a natural food colorant extracted from the seeds of the Bixa orellana L. plant. Annatto is used in Latin American cuisine to add a deep red color as well as distinctive flavor notes to fish, meat, and rice dishes. In the United States, annatto extracts are primarily used to impart orange/yellow hues to cheese and other dairy foods. The objective of this study was to identify and compare volatile compounds present in water- and oil-soluble annatto extracts. Volatile compounds were recovered using dynamic headspace-solvent desorption sampling and analyzed using GC-MS. Compounds were identified by comparison to a mass spectral database, Kovats indexes, and retention times of known standards. Of the 107 compounds detected, 56 compounds were tentatively identified and 51 were positively identified. Volatile profile differences exist between water- and oil- soluble extracts, and annatto extracts contain odorants with the potential to influence food aroma.  相似文献   

2.
Surface analysis of soil material by X-ray photoelectron spectroscopy   总被引:2,自引:0,他引:2  
The surface composition of particles present in the fine earth (< 2 mm) of 50 soil horizons differing in composition and pedogenetic origin (13 soil profiles) was analysed by X‐ray photoelectron spectroscopy (XPS) to assess the capability and limitations of this technique and to gain better knowledge of the soil samples. The surfaces were systematically enriched in carbon, sometimes up to 1000 times, indicating that the soil particle surfaces are coated with organic substances, even in horizons where the bulk organic content is less than 0.1 g kg?1. The distribution of carbon in the various oxidation states was 0.569 ± 0.008 C[0], 0.275 ± 0.004 C[+1], 0.089 ± 0.003 C[+2] and 0.066 ± 0.002 C[+3] for most horizons (mean ± standard error, 69 data). Only Andosol surface horizons systematically had surface organic matter in a more oxidized state. After correcting the results for the presence of organic coatings, we found that Si was generally depleted and Al enriched at the surface of soil particles, while Fe was either depleted or enriched depending on the sample considered. However, the coating of the coarser soil particles by the finer ones and their differential composition explained this observation and limits the interest of XPS for characterizing the surface enrichment of inorganic elements in crude soil samples. These limitations should be considered when interpreting XPS results in future work. Nevertheless, XPS can analyse the adsorbed organic matter and its functional composition of carbon without the need for any chemical or physical extraction that might alter the structure and composition of the organic molecules.  相似文献   

3.
The functional properties of wheat powders depend largely on the surface characteristics of their particles. X-ray photoelectron spectroscopy (XPS) has been considered to investigate the surface composition of wheat powders. The objective of the present study is to evaluate the ability of XPS to discriminate wheat components and to calculate the surface composition of wheat powders. First, XPS surveys for the main wheat isolated components (starch, proteins, arabinoxylans, and lipids) were determined. XPS results demonstrate that it is able to distinguish wheat proteins, polysaccharides, and lipids, but it is not able to distinguish starch and arabinoxylan because of their similarity in chemical structure. The XPS analyses of simple reconstituted wheat flours based on two components (starch and protein) or three components (by adding arabinoxylan) demonstrated the ability of XPS to measure the surface composition of the wheat flours. The surface composition of native wheat flour demonstrated an overrepresentation of protein (54%) and lipids (44%) and an underrepresentation of starch (2%) compared to the bulk composition. Results are discussed with regard to difficulties in discriminating arabinoxylans and starch components.  相似文献   

4.
Seeds, of either commercial crucifer crops or some wild and weed relatives, were screened for intact glucosinolates using a previously developed ion-pair LC-MS method. This method, in contrast to GC-MS techniques, ensures the accurate measurement of all classes of glucosinolates. Many crucifer seeds contained very high concentrations of glucosinolates with low concentrations of additional pigments and secondary metabolites. The other common seed metabolites were cinnamoylcholine esters, for example, sinapine. Glucosinolates derived from homologues of l-methionine were characteristic of Brassica and related crucifer species. In addition, significant concentrations of 4-hydroxy-3-indolylmethylglucosinolate were found in the majority of Brassica species. Wild and weed species often had relatively simple glucosinolate profiles: either a single glucosinolate or a predominant glucosinolate together with trace amounts of others. Species identified with seed glucosinolate profiles suitable for purification included various Alyssum, Erysimum, and Iberis species for 3-methythiopropyl-glucosinolate and 3-methylsulfinylpropyl-glucosinolate and various Alyssum, Erysimum, and Lepidium species with very high concentrations of C4-C6 aliphatic glucosinolates. Seeds of Arabis, Barbarea, Lepidium, Moringa, and Sinapis species were good sources of aromatic glucosinolates, and Azima tetracantha was a good source for N-methoxy-3-indolylmethyl-glucosinolate. MS data are reported for all of the intact glucosinolates detected from the screening process.  相似文献   

5.
Soils are structurally heterogeneous across a wide range of spatio-temporal scales. Consequently, external environmental conditions do not have a uniform effect throughout the soil, resulting in a large diversity of micro-habitats. It has been suggested that soil function can be studied without explicit consideration of such fine detail, but recent research has indicated that the micro-scale distribution of organisms may be of importance for a mechanistic understanding of many soil functions. Current techniques still lack the adequate sensitivity and resolution for data collection at the micro-scale, and the question ‘How important are various soil processes acting at different scales for ecological function?’ is therefore challenging to answer. The nano-scale secondary ion mass spectrometer (NanoSIMS) represents the latest generation of ion microprobes, which link high-resolution microscopy with isotopic analysis. The main advantage of NanoSIMS over other secondary ion mass spectrometers is its ability to operate at high mass resolution, whilst maintaining both excellent signal transmission and spatial resolution (down to 50 nm). NanoSIMS has been used previously in studies focussing on presolar materials from meteorites, in material science, biology, geology and mineralogy. Recently, the potential of NanoSIMS as a new tool in the study of biophysical interfaces in soils has been demonstrated. This paper describes the principles of NanoSIMS and discusses the potential of this tool to contribute to the field of biogeochemistry and soil ecology. Practical considerations (sample size and preparation, simultaneous collection of isotopes, mass resolution, isobaric interference and quantification of the isotopes of interest) are discussed. Adequate sample preparation, avoiding bias due to artefacts, and identification of regions-of-interest will be critical concerns if NanoSIMS is used as a new tool in biogeochemistry and soil ecology. Finally, we review the areas of research most likely to benefit from the high spatial and high mass resolution attainable with this new approach.  相似文献   

6.
This paper describes a rapid LC-MS/MS/MS method for the analysis of alpha-amanitin in serum and liver. Serum was initially prepared by precipitation of proteins with acetonitrile and subsequent removal of acetonitrile with methylene chloride. Liver was prepared by homogenization with aqueous acetonitrile and subsequent removal of acetonitrile using methylene chloride. For both matrices, the aqueous phase was then extracted using mixed-mode C18/cation exchange SPE cartridges and analyzed on a linear ion trap LC-MS system. Standards were prepared in extracts of control matrix. Seven replicate fortifications of serum at 0.001 mug/g (1 ng/g) of alpha-amanitin gave a mean recovery of 95% with 8.8% CV (relative standard deviation) and a calculated method detection limit of 0.26 ng/g. Seven replicates of control liver fortified at 1 ng/g gave a mean recovery of 98% with 17% CV and a calculated method detection limit of 0.50 ng/g. This is the first report of a positive mass spectrometric identification and quantitation of alpha-amanitin in serum and liver from suspect human and animal intoxications.  相似文献   

7.
The emergence of primary and secondary oxidation products in New Zealand extra virgin olive oil during accelerated thermal oxidation was measured and correlated with the concentrations of 13 headspace volatile compounds measured by selected ion flow tube mass spectrometry (SIFT-MS). SIFT-MS is a mass spectrometric technique that permits qualitative and absolute quantitative measurements to be made from whole air, headspace, or breath samples in real-time down to several parts per billion (ppb). It is well-suited to high-throughput analysis of headspace samples. Propanal, hexanal, and acetone were found at high concentrations in a rancid standard oil, while propanal, acetone, and acetic acid showed marked increases with oxidation time for the oils used in this study. A partial least-squares (PLS) regression model was constructed, which allowed the prediction of peroxide values (PV) for three separate oxidized oils. Sensory rancidity was also measured, although the correlations of headspace volatile compounds with sensory rancidity score were less satisfactory, and too few results were available for the construction of a PLS regression model. A fast (approximately 1 min), reliable method for prediction of olive oil PVs by SIFT-MS was developed.  相似文献   

8.
Seeds of melon (Citrullus lanatus var. sp.), pumpkin (Cucurbita moschata), and sunflower (Heliantus annus) were gamma-irradiated at 1, 3, 5, and 10 kGy and analyzed by electron paramagnetic resonance (EPR) and gas chromatography-mass spectrometry (GC-MS) according to EN1787:2000 and EN1785:2003, respectively. Distinguishable triplet signals due to the presence of induced cellulose radicals were found at 2.0010-2.0047 g in the EPR spectra. The gamma-irradiated radiolytic markers of 2-dodecylcyclobutanone (2-DCB) and 2-tetradecylcyclobutanone (2-TCB) were identified in all irradiated seed samples. Both the free radicals and the alkylcyclobutanones were found to increase with irradiation dose. In general, linear relationships between the amount of radicals and irradiation dosage could be established. Studies at an ambient temperature (20-25 degrees C) in a humidity-controlled environment showed a complete disappearance of the cellulosic peaks for irradiated samples upon 60 days of storage. Such instability behavior was considered to render the usefulness of using EPR alone in the determination of irradiated seed samples. On the other hand, 2-DCB and 2-TCB were also found to decompose rapidly (>85% loss after 120 days of storage), but the radiolytic markers remained quantifiable after 120 days of postirradiation storage. These results suggest that GC-MS is a versatile and complimentary technique for the confirmation of irradiation treatment to seeds.  相似文献   

9.
A gas chromatographic-single ion mass spectrometric method was developed for determining dimethoate residues in wheat plants. The base peak (m/e 37) of dimethoate was chosen as the single ion peak, and methyl stearate was used as an internal standard for this analysis. The minimum detectable concentration of dimethoate by this method was about 0.1 ppm for a 20 g wheat plant sample. The recoveries of dimethoate were about 89% at 0.13 ppm and greater than 96% at 0.5-1 ppm.  相似文献   

10.

Purpose

Antimony (Sb) contamination in the environment is a worldwide concern. To address such contamination issues, we studied the adsorption of Sb in four different types of soils. We investigated the main chemical and physical factors that influenced the adsorption of Sb, and distinguished between the different adsorption abilities of naturally occurring crystalline and amorphous iron (Fe) compounds in these soils.

Materials and methods

Adsorption of Sb in ferrosol, primosol, isohumosol, and sandy soil was studied using batch experiments. Transmission electron microscopy and X-ray photoelectron spectroscopy were used to examine the character and location of Sb adsorbed on individual particles in these soils without affecting its geochemical environment. In addition, the crystalline and amorphous Fe compounds in these soils were separated and analyzed using X-ray diffraction. The relationship between these Fe compounds and Sb adsorption was also explored.

Results and discussion

The sorption capacities of the four soils increased on addition of Sb in solution, reaching values of 10.8, 4.33, 5.45, and 1.19 g kg?1 for ferrosol, primosol, isohumosol, and sandy soil, respectively. The adsorption of Sb in ferrosol was much higher than for other soils because of its higher Fe oxide content. In fact, the Sb content adsorbed on ferrosol showed a good exponential relationship with its Fe content. The X-ray photoelectron spectroscopy results indicated that the Fe2p and O1s binding energies decreased after the adsorption of Sb in the ferrosol. This suggests that an electron transfer occurred between Sb and Fe through an oxidation-reduction reaction, after Sb adsorption in the ferrosol.

Conclusions

The adsorption abilities of Sb in the four soils were in the order of ferrosol > isohumosol > primosol > sandy soil. The amounts of Sb adsorbed by these soils were significantly positively correlated with their Fe contents (Sb?=??3.78?+?2.88?×?Fe, P?<?0.01), but were negatively correlated with their sand contents (Sb?=?12.30???0.12?×?Sand, P?<?0.01). The X-ray diffraction analysis results showed that crystalline Fe compounds have a higher capacity for Sb adsorption than amorphous Fe compounds.
  相似文献   

11.
In this work the quantitative determination and analytical speciation of arsenic were undertaken in different types of nuts, randomly purchased from local markets. The hardness of the whole nuts and high lipid content made the preparation of this material difficult for analysis. The lack of sample homogeneity caused irreproducible results. To improve the precision of analysis, arsenic was determined separately in nut oil and in the defatted sample. The lipids were extracted from the ground sample with the two portions of a mixture of chloroform and methanol (2:1). The defatted material was dried and ground again, yielding a fine powder. The nut oil was obtained by combining the two organic extracts and by evaporating the solvents. The two nut fractions were microwave digested, and total arsenic was determined by inductively coupled plasma mass spectrometry (ICP-MS). The results obtained for oils from different types of nuts showed element concentration in the range 2.9-16.9 ng g(-)(1). Lower levels of arsenic were found in defatted material (<0.1 ng g(-)(1) with the exception of Brazil nuts purchased with and without shells, 3.0 and 2.8 ng g(-)(1) respectively). For speciation analysis of arsenic in nut oils, elemental species were extracted from 2 g of oil with 12 mL of chloroform/methanol (2:1) and 8 mL of deionized water. The aqueous layer, containing polar arsenic species, was evaporated and the residue dissolved and analyzed by ion chromatography-ICP-MS. The anion exchange chromatography enabled separation of As(III), dimethylarsinic acid (DMAs(V)), monomethylarsonic acid (MMAs(V)), and As(V) within 8 min. Several types of nuts were analyzed, including walnuts, Brazil nuts, almonds, cashews, pine nuts, peanuts, pistachio nuts, and sunflower seeds. The recovery for the speciation procedure was in the range 72.7-90.6%. The primary species found in the oil extracts were As(III) and As(V). The arsenic concentration levels in these two species were 0.7-12.7 and 0.5-4.3 ng g(-)(1), respectively. The contribution of As in DMAs(V) ranged from 0.1 +/- 0.1 ng g(-)(1) in walnuts to 1.3 +/- 0.3 ng g(-)(1) in pine nuts. MMAs(V) was not detected in almonds, peanuts, pine nuts, sunflower seeds, or walnuts, and the highest concentration was found in pistachio nuts (0.5 +/- 0.2 ng g(-)(1)).  相似文献   

12.
为实现对新陈莲子的快速鉴别,该文采用自行研制的表面解吸常压化学电离质谱(DAPCI-MS),在无需样品预处理的前提下,直接对新鲜和陈年莲子切面进行质谱检测,获得其化学指纹图谱,并通过主成分分析(PCA)和反向传输人工神经网络技术(BP-ANN)对所获指纹谱图信息进行分析,获得新鲜和陈年莲子的质谱信息特征。结果表明,在负离子模式下,DAPCI-MS结合化学计量学方法,实现了新鲜和陈年莲子的快速鉴别,其测试样本准确率分别为95.0%和91.7%;对不同年份莲子也能够有效地分类判别,2012、2011、2010和2009年莲子测试样本准确率分别为90%,85%,85%和90%。该方法具有分析速度快,信息提取准确,识别精度高等优点,为其他粮食谷物品质的鉴定提供参考。  相似文献   

13.
Phenyl urea herbicides were determined in water by electrospray quadrupole ion trap liquid chromatography-mass spectrometry (ES-QIT-LC-MS). Over a wide concentration range [M - H](-) and MH(+) ions were prominent in ES spectra. At high concentrations dimer and trimer ions appeared, and sodium, potassium, and ammonium adducts also were observed. In the case of isopturon, source collision-induced dissociation (CID) fragmentation with low offset voltages increased the ion current associated with MH(+) and diminished dimer and trimer ion abundance. In the mass analyzer CID involved common pathways, for example, daughter ions of [M - H](-) resulted from loss of R(2)NH in N',N'-dialkyl ureas or loss of C(3)H(5)NO(2) (87 amu) in N'-methoxy ureas. A 2 mm (i.d.) x 15 cm C(18) reversed phase column was used for LC-MS with a linear methanol/water gradient and 0.5 mL/min flow rate. Between 1 and 100 pg/microg/L the response was highly linear with instrument detection limits ranging from <10 to 50 pg injected. Whereas the positive ES signal intensity was greater for each of the compounds except fluometuron, negative ion monitoring gave the highest signal-to-noise ratio. Analysis of spiked Colorado River water, a source high in total dissolved solids and total organic carbon, demonstrated that ES-QIT-LC-MS was routinely capable of quantitative analysis at low nanogram per liter concentrations in conjunction with a published C(18) SPE method. Under these conditions experimental method detection limits were between 8.0 and 36 ng/L, and accuracy for measurements in the 20-50 parts per trillion range was from 77 to 96%. Recoveries were slightly lower in surface water (e.g., 39-76%), possibly due to suppression of ionization.  相似文献   

14.
A method was developed to determine pesticides in malt beverages using solid phase extraction on a polymeric cartridge and sample cleanup with a MgSO4-topped aminopropyl cartridge, followed by capillary gas chromatography with electron impact mass spectrometry in the selected ion monitoring mode [GC-MS(SIM)]. Three GC injections were required to analyze and identify organophosphate, organohalogen, and organonitrogen pesticides. The pesticides were identified by the retention times of peaks of the target ion and qualifier-to-target ion ratios. GC detection limits for most of the pesticides were 5-10 ng/mL, and linearity was determined from 50 to 5000 ng/mL. Fortification studies were performed at 10 ng/mL for three malt beverages that differ in properties such as alcohol content, solids, and appearance. The recoveries from the three malt beverages were greater than 70% for 85 of the 142 pesticides (including isomers) studied. The data showed that the different malt beverage matrixes had no significant effect on the recoveries. This method was then applied to the screening and analysis of malt beverages for pesticides, resulting in the detection of the insectide carbaryl and the fungicide dimethomorph in real samples. The study indicates that pesticide levels in malt beverages are significantly lower than the tolerance levels set by the United States Environmental Protection Agency for malt beverage starting ingredients. The use of the extraction/cleanup procedure and analysis by GC-MS(SIM) proved effective in screening malt beverages for a wide variety of pesticides.  相似文献   

15.
Carbohydrates in commercial tobacco products were quantified utilizing a liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS) technique. The method utilizes negative ion electrospray with multiple reactions monitoring and an internal standard calibration. Snuffs, chewing tobaccos, cigars, and cigarettes were analyzed. Product type differentiation was possible using the carbohydrate levels coupled with pH and moisture contents. The LC-MS/MS method was compared to a method utilizing ion chromatography with pulsed amperometric detection. The LC-MS/MS method provided improved selectivity and specificity, demonstrated better precision, and had a larger dynamic range for glucose, fructose, and sucrose in tobacco extracts.  相似文献   

16.
A method is presented for the quantification and structure confirmation of trichothecenes in wheat by high-performance liquid chromatography combined with multiple mass spectrometry (MS(n)()). Nine type A- and B-trichothecenes were determined (nivalenol, deoxynivalenol, fusarenon-X, 3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol, neosolaniol, diacetoxyscirpenol, HT-2 toxin, and T-2 toxin). Extraction was carried out with acetonitrile/water. The extract was purified on a MycoSep column. Quantification was based on an internal standard and atmospheric pressure chemical ionization in the positive ion mode. Recoveries from spiked wheat were in the range of 80-106% at levels of 500 ppb. The limits of quantification for the whole method were between 10 and 100 ppb. Ion adduct formation with ammonium and acetate ions and MS(n) experiments provided information about substitution and fragmentation behavior of the mycotoxins. A scheme has been established for the partial structure elucidation of type A- and B-trichothecenes in fungal cultures.  相似文献   

17.
A sample preparation method was developed to quantify environmentally relevant (low micrograms per liter) concentrations of perchlorate (ClO4(-)) in leafy vegetables using IC-ESI-MS. Lettuce and spinach were macerated, centrifuged, and filtered, and the aqueous extracts were rendered water-clear using a one-step solid-phase extraction method. Total time for extraction and sample preparation was 6 h. Ion suppression was demonstrated and was likely due to unknown organics still present in the extract solution after cleanup. However, this interference was readily eliminated using a Cl(18)O4(-) internal standard at 1 microg/L in all standards and samples. Hydroponically grown perchlorate-free butterhead lettuce was spiked to either 10.3 or 37.7 microg/kg of fresh weight (FW), and recoveries were between 91 and 98% and between 93 and 101%, respectively. Five types of lettuce and spinach from a local grocery store were then analyzed; they contained from 0.6 to 6.4 microg/kg of FW. Spike recoveries using the store-bought samples ranged from 89 to 100%. The method detection limit for perchlorate in plant extracts is 40 ng/L, and the corresponding minimum reporting limit is 200 ng/L or 0.8 microg/kg of FW.  相似文献   

18.
The ion trap detector (ITD), in combination with a capillary gas chromatograph and under chemical ionization conditions, offers sufficient sensitivity to determine carbadox-related residues as the methyl ester derivative of quinoxaline-2-carboxylic acid at 3 micrograms/kg or higher in porcine liver. A tetradeuterated internal standard of QME effectively compensates for losses incurred during sample preparation. The method produced mean levels of 3.3 (+/- 0.5), 5.5 (+/- 0.8), and 10.1 (+/- 0.9) micrograms/kg for liver fortified at 3, 5, and 10 micrograms/kg. When applied to analysis of samples containing incurred residues of 14C-carbadox at the low microgram/kg level, results were comparable to those obtained by reverse isotope dilution analysis.  相似文献   

19.
Extracts from 4 types of swine feed containing 0.11 ppm each of dimetridazole (DMZ) and ipronidazole (IPR) were analyzed by capillary gas chromatography/mass spectrometry (GC/MS) using multiple ion detection (MID) techniques. We demonstrate in this paper that the quantitative results obtained by capillary GC/MS with MID are comparable for both compounds to results obtained by liquid chromatography and have a lower coefficient of variation for DMZ. Moreover, consistency in the ion ratios (5 ions in DMZ and 6 ions in IPR) permits identification of these compounds by electron ionization MS.  相似文献   

20.
There is at present little information on the long‐term stability of phosphorus sequestered in wetlands. Phosphorus sequestered during high loading periods may be relatively unstable and easily remobilized following changes in nutrient status or hydrological regime, but the chemical forms of sequestered phosphorus that do remobilize are largely unknown at this time. A lack of suitable analytical techniques has contributed to this dearth of knowledge regarding the stability of soil organic phosphorus. We analysed phosphorus in soils from the ‘head’ of Rescue Strand tree island and an adjacent marsh in the Florida Everglades by 31P nuclear magnetic resonance (NMR) spectroscopy and high‐resolution mass spectrometry. Tree islands are important areas of biodiversity within the Everglades and offer a unique opportunity to study phosphorus sequestration because they are exposed to large phosphorus loads and appear to be natural nutrient sinks. The 31P NMR profiling of extracts from surface and sediment samples in the tree island indicates that phosphorus input to Rescue Strand tree island soils is mostly in the form of inorganic ortho‐phosphate and is either refractory when deposited or rapidly recycled by the native vegetation into a stable phosphorus pool largely resistant to re‐utilization by plants or microbes. Mass spectrometry revealed the presence of inositol hexakisphosphate, a common organic monophosphate ester not previously observed in Everglades’ soils.  相似文献   

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