Cloud point extraction preconcentration prior to high-performance liquid chromatography coupled with cold vapor generation atomic fluorescence spectrometry for speciation analysis of mercury in fish samples

A cloud point extraction methodology was developed for simultaneous preconcentration of Hg(II), methylmercury (MeHg), ethylmercury (EtHg), and phenylmercury (PhHg) prior to reversed-phase high-performance liquid chromatography (HPLC) on-line coupled with cold vapor atomic fluorescence spectrometry for speciation analysis of mercury in fish. The four mercury species were taken into complexes with ammonium pyrrolidine dithiocarbamate (APDC) in aqueous nonionic surfactant Triton X-114 medium and concentrated in the surfactant-rich phase by bringing the solution to the temperature of 40 degrees C. Baseline separation of the enriched complexes was achieved on an RP-C(18) column with a mixture of methanol, acetonitrile, and water (65:15:20, v/v) containing 200 mmol L(-1) HAc (pH 3.5) as the mobile phase. An on-line postcolumn oxidation of the effluent from HPLC, in the presence of K2S2O8 in HCl, was applied in the system followed by an optimal cold vapor generation of mercury species. The variables affecting the complexation and extraction steps were examined. The preconcentration of 10 mL of solution with 0.08% w/v Triton X-114 and 0.04% w/v APDC at pH 3.5 gave enrichment factors of 29, 43, 80, and 98 for MeHg, EtHg, PhHg, and Hg(II), respectively. Low detection limits (S/N = 3) were obtained, ranging from 2 to 9 ng L(-1) (as Hg) for all species. The developed method was successfully applied to the speciation of mercury in real fish samples.     

Rapid and sensitive determination of sulfonamide residues in milk and chicken muscle by microfluidic chip electrophoresis

A new, rapid, and sensitive method was proposed for the determination of sulfonamide residues in milk and chicken muscle samples by microchip electrophoresis with laser-induced fluorescence detection. Separation of fluorescamine-labeled sulfonamides was accomplished by using a buffer containing 5 mmol/L boric acid and 1% (w/v) polyvinyl alcohol (PVA). The pH, amount of PVA, and concentration of boric acid in the running buffer were found to have great influence on the separation. By optimizing these conditions, the separation of four sulfonamides, sulfamethazine, sulfamethoxazole, sulfaquinoxaline, and sulfanilamide, was achieved within 1 min with limits of detection (S/N = 3) of 0.2-2.3 μg/L, which are well below the maximum residue limit. The proposed method also exhibited very good repeatability; the relative standard deviations for both within-day and between-day measurements were ≤3.0%. With a simplified sample pretreatment protocol, fast determination of sulfonamides in real samples was successfully performed with standard addition recoveries of 93.3-100.8 and 82.9-92.3%, respectively.     

Simultaneous determination of ochratoxin A and cyclopiazonic,mycophenolic, and tenuazonic acids in cornflakes by solid-phase microextraction coupled to high-performance liquid chromatography

A solid-phase microextraction (SPME) method, coupled to liquid chromatography with diode array UV detection (LC-UV/DAD), for the simultaneous determination of cyclopiazonic acid, mycophenolic acid, tenuazonic acid, and ochratoxin A is described. Chromatographic separation was achieved on a propylamino-bonded silica gel stationary phase using acetonitrile/methanol/ammonium acetate buffer mixture (78:2:20, v/v/v) as mobile phase. SPME adsorption and desorption conditions were optimized using a silica fiber coated with a 60 microm thick polydimethylsiloxane/divinylbenzene film. Estimated limits of detection and limits of quantitation ranged from 3 to 12 ng/mL and from 7 to 29 ng/mL, respectively. The method has been applied to cornflake samples. Samples were subjected to a preliminary short sonication in MeOH/2% KHCO(3) (70:30, v/v); the mixture was evaporated to near dryness and reconstituted in 1.5 mL of 5 mM phosphate buffer (pH 3) for SPME followed by LC-UV/DAD. The overall procedure had recoveries (evaluated on samples spiked at 200 ng/g level) ranging from 74 +/- 4 to 103 +/- 9%. Samples naturally contaminated with cyclopiazonic and tenuazonic acids were found; estimated concentrations were 72 +/- 9 and 25 +/- 6 ng/g, respectively.     

Fast determination of Sudan dyes in chilli tomato sauces using partial filling micellar electrokinetic chromatography

A new method based on partial filling micellar electrokinetic chromatography (MEKC) for the quantitative determination of Sudan dyes (I, II, III, and IV) in chilli sauces is presented. The separation is achieved filling 25% of the capillary with a MEKC buffer composed of 40 mM NH(4)HCO(3), 25 mM sodium dodecyl sulfate, and 32.5% (v/v) acetonitrile (ACN). The rest of the capillary is filled using a capillary zone electrophoresis (CZE) buffer composed of 40 mM NH(4)HCO(3) and 32.5% (v/v) ACN. Under optimized conditions, the azo dyes are baseline separated in less than 8 min with limits of detection ranging from 0.57 to 0.71 μg mL(-1) (S/N > 3). Using an internal standard, the repeatability of the quantitative determination is improved almost four times. The applicability of the method for rapid screening and determination of Sudan dyes is corroborated by analyzing spiked chilli sauce samples with recoveries from 85 to 99%. The reported conditions are demonstrated to be compatible with mass spectrometry detection.     

Acidity and conductivity of precipitation on central Long Island,New York in relation to meteorological variables

Three years of hourly sequential precipitation samples from central Long Island, New York were analyzed to determine the relationships between acidity and conductivity and concentrations of sulfate, nitrate plus nitrite, nitrogen in ammonium, sodium, and chloride ions. Relationships between precipitation acidity and meteorological conditions were also studied. Hydrogen ion concentrations are similar to those elsewhere in the northeastern United States. They are best correlated with sulfate concentrations but also correlate with concentrations of nitrogen in nitrate plus nitrite and nitrogen in ammonium ion. Concentrations are highest in the summer, with cold front and squall line precipitation and with rain showers and thundershowers. All ions measured contributed to sample conductivity but hydrogen ion contributed the most with sulfate ion second. Conductivity calculated from concentrations of the separate ions agreed well with measured conductivity. Conductivity showed relationships to meteorological conditions similar to those of hydrogen ion concentration except when sodium and chloride ions predominated in the sample.     

Kale carotenoids are unaffected by, whereas biomass production, elemental concentrations, and selenium accumulation respond to, changes in selenium fertility

Selenium (Se) is a micronutrient in mammalian nutrition and is accumulated in kale (Brassica oleracea L. var. acephala), which has high levels of lutein and beta-carotene. Selenium, lutein, and beta-carotene have important human health benefits and possess strong antioxidant properties. The objectives of this study were to determine the influence of different Se [as sodium selenate (Na(2)SeO(4)) and sodium selenite (Na(2)SeO(3))] fertility levels on (1) biomass accumulation, (2) the accumulation patterns of carotenoid pigments, and (3) elemental accumulation in the leaves of kale. Winterbor kale was greenhouse-grown using nutrient solution culture with Se treatment concentrations of 0.0, 0.5, 1.0, 1.5, 2.0, 2.5, 3.0, and 3.5 mg Se/L as Na(2)SeO(4) and 0.0, 0.5, 1.0, 1.5, 2.0, 2.5, and 3.0 mg Se/L as Na(2)SeO(3). Increases in either selenate (SeO(4)(-)(2)) or selenite (SeO(3)(-)(2)) resulted in decreases in kale leaf tissue biomass. Neither of the Se treatments had an effect on the accumulation of lutein or beta-carotene in leaf tissues. Increasing SeO(4)(-)(2) significantly increased the accumulation of kale leaf Se; however, leaf tissue Se did not significantly change over the SeO(3)(-)(2) treatments. Increases in SeO(4)(-)(2) affected the leaf tissue concentrations of P, K, Ca, Mg, S, B, Cu, Mn, and Mo, whereas SeO(3)(-)(2) only affected B and S. Growing kale in the presence of SeO(4)(-)(2) would result in the accumulation of high levels of tissue Se without affecting carotenoid concentrations.     

Simultaneous determination of five plant growth regulators in fruits by modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction and liquid chromatography-tandem mass spectrometry

An effective method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed and optimized to obtain a complete separation of five representative plant growth regulators (PGRs) [gibberellic acid, 2,4-dichlorophenoxyacetic acid (2,4-D), thidiazuron, forchlorfenuron, and paclobutrazol] in fruits. Extraction was performed with acetonitrile containing 0.1% (v/v) acetic acid, applying modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) methodology. LC-MS/MS conditions including composition of mobile phases and mass spectrometry (MS) conditions were evaluated to achieve the highest sensitivity in MS detection. All of the data acquisition was employed in the segmented multiple-reaction monitoring mode for the selected negative and positive transition ions. The octadecylsilyl (C18) dispersive solid-phase extraction (SPE) sorbent was found to provide the more satisfied recoveries than primary secondary amine (PSA) and graphitized carbon black (GCB) for five target PGRs. The optimized method allowed for recoveries of 76-112% for the five PGRs from fruit samples with relative standard deviation (RSD) values less than 10%. Limits of quantification (0.5-16.5 μg/kg) were lower than the maximum limit of residues established for PGRs. The results demonstrated that the developed LC-MS/MS and QuEChERS extraction method is highly effective for analyzing trace amounts of target PGRs in fruit samples. Finally, the method was successfully used to detect residual PGRs in Beijing, China, in 2010. The concentrations of 2,4-D (5.1-1503 μg/kg) and paclobutrazol (1-1381 μg/kg) found in orange and peach, respectively, suggesting that the use of these PGRs in these fruits should be regulated in China in the future.     

Determination of ascorbic acid and carotenoids in food commodities by liquid chromatography with mass spectrometry detection

Two methods, one to determine ascorbic acid and one to determine lycopene and beta-carotene, in vegetables and fruits by liquid chromatography coupled with mass spectrometry (LC-MS) have been established. The chromatographic separation of the studied compounds and their MS parameters were optimized to improve selectivity and sensitivity. In both methods, separation was carried out with two coupled columns, first a C(18) and then a dC(18), using as mobile phase 70% methanol (0.005% acetic acid) and 30% acetic acid 0.05% for ascorbic acid determination and a mixture of methanol, tetrahydrofuran, and acetonitrile (60:30:10 v/v/v) for carotenoid analysis in isocratic mode. The molecular ion was selected for the quantification in selective ion monitoring (SIM) mode. Ascorbic acid was detected with electrospray ionization probe (ESI) in negative mode, while chemical ionization atmospheric pressure (APCI) in positive mode was used for the target carotenoids. The methodology for ascorbic acid analysis is based on an extraction with polytron using methanol and a mixture of methaphosphoric acid and acetic acid. Extraction of the carotenoids was carried out with tetrahydrofuran/methanol (1:1) (v/v). The proposed methods were applied, after their corresponding validations, to the analysis of four varieties of tomatoes, tomato in tin enriched and dried tomato, and to the analysis of mango and kiwi fruits, to compare the content in these compounds. Moreover, the influence of the process of freezing and the effect that the manipulation/preservation has in the content of ascorbic acid in tomato have also been studied.     

Hydrogen ion input to the hubbard brook experimental forest,New Hampshire,during the last decade

Being downwind of eastern and midwestern industrial centers, the Hubbard Brook Experimental Forest offers a prime location to monitor long-term trends in atmospheric chemistry. Continuous measurements of precipitation chemistry during the last 10 yr provide a measure of recent changes in precipitation inputs of H ion. The weighted average pH of precipitation during 1964–65 to 1973–74 was 4.14, with a minimum annual value of 4.03 in 1970–71 and a maximum annual value of 4.21 in 1973–74. The sum of all cations except H ion decreased from 51 μeq 1^?1 in 1964–65 to 23 μeq 1^?1 in 1973–74 providing a significant drop in neutralizing capacity during this period. Based upon regression analysis, the input in equivalents of H ion and nitrate increased by 1.4-fold and 2.3-fold respectively, from 1964–65 to 1973–74. Input of all other ions either decreased or showed no trend. Based upon a stoichiometric formation process in which a sea-salt, anionic component is subtracted from the total anions in precipitation, SO₄ ⁼, contribution to acidity dropped from 83% to 66%, whereas NO₃ ^? increased from 15% to 30% during 1964–65 to 1973–74. The increased annual input of H ion at Hubbard Brook during the past 10 yr is highly correlated with the increased input of nitrate in precipitation.     

恒电荷土壤及可变电荷土壤与离子间相互作用的研究 I.共存离子对NO_3~-吸附的影响

研究了我国典型３种可变电荷土壤和４种恒电荷土壤在陪伴阳离子分别为Ｋ十、Ｎａ十、Ｃａ２＋时和１ｍｍｏｌＬ－１ＫＣ１、Ｋ２ＳＯ４支持电解质中ＮＯ３－的吸附。结果表明，ＮＯ３－吸附量随ｐＨ的增加而减小。在添加相同浓度ＮＯ３－时，３种可变电荷土壤对ＮＯ３－的吸附量顺序为Ｃａ（ＮＯ３）２＞ ＫＮＯ３＞ＮａＮＯ３＞ＫＮＯ３十ＫＣＩ＞ＫＮＯ３＋Ｋ２ＳＯ４；在初始ＮＯ３－浓度０．５－５ｍｍｏｌＬ－１的范围内，吸附量随浓度变化的关系符合Ｌａｎｇｍｕｉｒ等温吸附式．由此求出与ＮＯ３－吸附结合能有关的常数（Ｋ）在不同共存离子存在下数值较小且差异不大，因此认为不同陪伴阳离子和不同伴随阴离子对ＮＯ３－吸附的电性机理影响不大，只是改变了土壤表面的正电荷数量从而使吸附量发生变化。４种恒电荷土壤对ＮＯ３－的吸附量通常很小，其中在Ｃａ（ＮＯ３）２介质中较在其他介质中稍大，最大吸附量仅为１．５～ｍｍｏｌ ｋｇ－１左右，约为可变电荷土壤的１／１０，且在浓度较低时常观察到负吸附。     

Development of an analytical method for the determination of beta2-agonist residues in animal tissues by high-performance liquid chromatography with on-line electrogenerated [Cu(HIO6)2]5- -luminol chemiluminescence detection

A novel method was developed for the simultaneous determination of beta2-agonist residues such as terbutaline, salbutamol, and clenbuterol by high-performance liquid chromatography (HPLC) coupled with chemiluminescence (CL) detection. The procedure was based on the enhancement effect of beta2-agonists on the CL reaction between luminol and the complex of trivalent copper and periodate ([Cu(HIO6)2]5-), which was on-line electrogenerated by constant current electrolysis. The HPLC separation used a Nucleosil RP-C18 column (250 mm x 4.6 mm i.d., 5 microm; pore size, 100 A) with a mobile phase consisting of 90% acetonitrile and 10% aqueous ammonium acetate (20 mmol L-1, pH 4.0) at a flow rate of 1.0 mL min-1. The effects of several parameters on the HPLC resolution and CL emission were studied systematically. Liver samples were hydrolyzed with beta-glucuronidase followed by a solid-phase extraction procedure using Waters OasisMCX cartridges. Under optimum conditions, the limits of detection at a signal-to-noise ratio of 3 ranged from 0.007 to 0.01 ng g-1 and the limits of quantification at a signal-to-noise ratio of 10 ranged from 0.023 to 0.033 ng g-1 for three beta2-agonists. The relative standard deviations (RSDs) of intra- and interday precision were below 4.5%. The average recoveries for beta2-agonists (spiked at the levels of 0.05-5.0 ng g-1) in pig liver ranged from 84 to 110%, and the RSDs of the quantitative results were from 1.6 to 7.2%. The proposed method was successfully applied to the determination of beta2-agonist residues in pig liver samples.     

Simultaneous Determination of Furostanol, Pennogenyl, and Diosgenyl Glycosides in Taiwanese Rhizoma Paridis ( Paris formosana Hayata) by high-performance liquid chromatography with evaporative light scattering detection

A high-performance liquid chromatographic method with an evaporative light scattering detector (HPLC-ELSD) was developed to simultaneously determine 10 steroidal saponins, including 3 furostanol glycosides, 3 pennogenyl glycosides, and 4 diosgenyl glycosides in Taiwanese rhizoma paridis ( Paris formosana Hayata). The condition was a Cosmosil C18 column kept at 35 °C and a step-gradient solvent system consisting of acetonitrile and water (25:75, v/v) in the first 30 min, 45:55 (v/v) from 31 to 45 min, and 50:50 (v/v) from 45 to 65 min, at a flow rate of 1 mL/min. The separation factors (α) and resolutions (Rs) were better than 1, and the limits of detection (LODs) and limits of quantification (LOQs) were 0.01-0.27 and 0.04-0.90 μg, respectively, for these saponins. Moreover, 203 nm UV detection was also used for comparison. The saponins in P. formosana Hayata gathered from various areas of Taiwan were determined by applying the established method.     

Direct and selective flow-injection method for the simultaneous spectrophotometric determination of calcium and magnesium in red and white wines using online dilution based on "Zone Sampling".

The present work reports a selective and simple flow injection method for the direct and simultaneous determination of calcium and magnesium ions in red, rose, and white wines. Both ions react with methylthymol blue (MTB) at a strongly basic medium to form colored complexes that are monitored spectrophotometrically (lambda(max) = 610 nm). The simultaneous determination is achieved by online masking of magnesium by 8-hydroxyquinoline (8-HQ). Incorporating an online dilution mode based on the "zone sampling" technique in the FI system, the determination of both analytes was achieved without any pretreatment of the samples, in the range 0-350 mg L(-1) and 0-200 mg L(-1) for Ca(II) and Mg(II), respectively. The 3 sigma detection limits were quite satisfactory (2.1 and 1.8 mg L(-1) for Ca(II) and Mg(II) respectively), and the precision was 1.2% (at a mixture of 100.0 mg L(-1) Ca(II) + 100.0 mg L(-1) Mg(II), n = 12). A detailed study of interferences proved that the proposed method is highly selective. The application of the method to the direct analysis of red, rose, and white wines yielded excellent results compared with those obtained by using FAAS as a reference method (e(r) < 2.8%).     

Extraction and separation of water-soluble proteins from different wheat species by acidic capillary electrophoresis

Optimization of protein extraction and a capillary zone electrophoresis method for water-soluble protein analysis in wheat is described. The optimal separation was obtained with a 50 microm i.d. x 27 cm (20 cm to detector) uncoated capillary filled with 0.1 M phosphoric acid/beta-alanine, pH 2.5, buffer containing urea (1 M), 0.05% (w/v) hydroxypropylmethylcellulose, and 20% (v/v) acetonitrile. Separation was carried out at 15 kV and 35 degrees C for 9 min. Extract stability was also investigated within 2 h from the extraction. Good visual peak parameters and a higher sensitivity can be obtained when 30% ethanol is used as an extraction medium. The method was successfully used to analyze extracts obtained from whole and refined meals of six Triticum spp. Moreover, the described methodology could be applied to the discrimination of species with different ploidy levels and to the detection of durum wheat adulteration, as well as to screen wheat collections for enzymes involved with the quality of wheat derivatives.     

High pressure liquid chromatographic determination of zearalenone in chicken tissues

A method is reported for the extraction and analysis of zearalenone in chicken fat, heart muscle, and kidney tissue by using high pressure liquid chromatography (HPLC). Zearalenone is extracted with acetonitrile, cleaned up with hexane, and extracted further with ethyl acetate. Zearalenone is determined by HPLC using a reverse phase radial compression separation system, an ultraviolet absorbance detector, and a mobile phase of acetonitrile-water (60 + 40) (v/v). Recoveries of zearalenone added at levels from 50 to 200 ng/g are in the range 82.6-95.1%.     

Dehydrotomatine and alpha-tomatine content in tomato fruits and vegetative plant tissues

Tomato plants (Lycopersicon esculentum) synthesize the glycoalkaloids dehydrotomatine and alpha-tomatine, possibly as a defense against bacteria, fungi, viruses, and insects. We used a high-performance liquid chromatography method with UV detection at 208 nm for the analysis of these compounds in various tissues. An Inertsil ODS-2 column with a mobile phase of acetonitrile/20 mM KH2PO4 (24/76, v/v) afforded good separation of the two glycoalkaloids in mini-tomato extracts, fruit harvested at different stages of maturity, and calyxes, flowers, leaves, roots, and stems. The two peaks appeared at approximately 17 and approximately 21 min. Recoveries from tomato fruit extracts spiked with dehydrotomatine and alpha-tomatine were 87.7 +/- 6.8 and 89.8 +/- 3.4% (n = 5), respectively. The detection limit is estimated to be 0.39 microg for dehydrotomatine and 0.94 microg for alpha-tomatine. The dehydrotomatine and alpha-tomatine content of tomatoes varied from 42 to 1498 and 521 to 16 285 microg/g of fresh weight, respectively. The ratio of alpha-tomatine to dehydrotomatine ranged from 10.9 to 12.5 in tomatoes and from 2.3 to 7.8 in the other plant tissues. These results suggest that the biosynthesis of the glycoalkaloids is under separate genetic control in each plant part. Degradation of both glycoalkaloids occurred at approximately the same rate during maturation of the tomatoes on the vine. An Inertsil NH2 column, with acetonitrile/1 mM KH2PO4 (96/4, v/v) as the eluent, enabled the fractionation of commercial tomatidine into tomatidenol and tomatidine, the aglycons of dehydrotomatine and alpha-tomatine, respectively. The information should be useful for evaluating tomatoes and vegetative tissues for dehydrotomatine/alpha-tomatine content during fruit development and their respective roles in host-plant resistance and the diet.     

Evaluation of dry ashing in conjunction with ion chromatographic determination of transition metal ions in pig feed samples

The contents of transition metal ions iron, copper, zinc, and manganese were simultaneously determined in pig feed using an ion chromatographic technique (IC) preceded by dry ashing. Employing ion exchange, the ions were separated on an IonPac CS5A column used in combination with a pyridine-2,6-dicarboxylic acid based eluent. The separation was followed by spectrophotometric detection after postcolumn reaction with 4-(2-pyridylazo)resorcinol. Dry ashing parameters were varied to assess their role in potential analyte loss. Quantitative recoveries (>95%) were obtained for all analytes with a dry ashing method that included a moderate temperature-time regime and ash leaching support in the form of sonication and heat treatment. The use of HCl as leaching acid and the presence of alkaline earths in the matrix solution did not interfere with the chromatographic separation.     

Separation and purification of tricin from an antioxidant product derived from bamboo leaves

Tricin (5,7,4'-trihydroxy-3',5'-dimethoxyflavone) occurs in its glycosidic form in rice bran and other grass species such as wheat, barley, and maize. Tricin is considered sufficiently safe for clinical development as a cancer chemopreventive agent, therefore it can be used for cancer prevention. This study established a new method for the preparation of tricin from bamboo leaves as an alternative to traditional methods such as chemical synthesis via the Baker-Venkata-Raman reaction between acetylsyringic acid and phloroacetophenone. Tricin was prepared from an antioxidant product that was derived from bamboo leaves (AOB) by extraction with aqueous ethanol. A concentrated solution of this product was obtained and then processed by polystyrene (AB-8) resin column chromatography and preparative high-performance liquid chromatography (HPLC) with 30% (v/v) acetonitrile in 1% (v/v) acetic acid as the mobile phase. The collected tricin-rich fraction was further sequentially purified by dialysis membrane separation and drowning-out crystallization methods. The purity was assessed by analytical HPLC with 25% (v/v) acetonitrile in 1% (v/v) acetic acid as the mobile phase, and the chemical confirmation was evaluated by infrared, mass, nuclear magnetic resonance, and ultraviolet spectroscopies. Tricin (3.09 g) was prepared from 174 g of a crude column chromatography fraction obtained from 5 L of AOB concentrated solution. The present method is appropriate for preparing quantities of pure tricin, which can be used for the quantification of tricin in various plant herbs and further for pharmaceutical/biomedical applications and evaluation.     

紫色土坡耕地硝态氮的迁移流失规律及其数值模拟

为探究紫色土坡耕地硝态氮迁移流失过程,通过室内模拟试验,并结合数学模型,研究在不同雨强(0.4,1.0,1.8 mm/min)和坡度(5?,15?,20?)下硝态氮分别随地表径流和壤中流迁移而流失的特征。结果表明:随地表径流和壤中流迁移的硝态氮流失浓度随时间分别呈现指数下降和线性上升趋势;随壤中流流失的浓度是地表径流携带的19~72倍,在小雨强下壤中流携带流失负荷大于随地表径流流失负荷,但随雨强增大,硝态氮流失负荷通过地表径流流失的比例由17.3%增大至66.0%,大雨强下硝态氮主要通过地表径流流失;与实测数据比较分析,有效混合深度模型在随地表径流流失的硝态氮模拟中精度评价指标Nash-Suttcliffe系数ENS和决定系数R2达到0.590和0.826 7,而对流弥散方程在壤中流携带硝氮流失的过程模拟中ENS和R2达到0.792和0.842 6,取得较好的模拟结果。该研究为紫色土坡耕地硝态氮迁移流失机理研究提供依据和参考。     

Separation of Delta5- and Delta7-phytosterols by adsorption chromatography and semipreparative reversed phase high-performance liquid chromatography for quantitative analysis of phytosterols in foods

A method for the separation, isolation, and identification of phytosterols was developed. A commercial phytosterols mixture, Generol 95S, was fractionated first by adsorption silica gel column chromatography and then separated by means of a semipreparative reverse phase high-performance liquid chromatography fitted with a Polaris C8-A column (250 mm x 10 mm i.d., 5 microm) using isocratic acetonitrile:2-propanol:water (2:1:1, v/v/v) as the mobile phase. Milligram scales of six individual phytosterols, including citrostadienol, campesterol, beta-sitosterol, Delta7-avenasterol, Delta7-campesterol, and Delta7-sitosterol, were obtained. Purities of these isolated sterols were 85-98%. Relative response factors (RRF) of these phytosterols were calculated against cholestanol as an authentic commercial standard. These RRF values were used to quantify by gas chromatography-mass spectrometry (GC-MS) the phytosterols content in a reference material, oils, and chocolates.