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1.
为探索利用高效液相色谱法测定设施番茄土壤低分子量有机酸的适宜色谱条件,以Na OH和Na Cl混合溶液为提取剂提取11种土壤低分子量有机酸,通过优化影响低分子量有机酸分离度的流动相浓度、p H、流速、有机改良剂的添加比例、检测波长等条件,确定了高效液相色谱法测定设施番茄土壤低分子量有机酸的最佳色谱条件为:以10 mmol L-1KH_2PO_4-CH_3OH(97∶3,p H 2.6)为流动相,流速为0.8 ml min~(-1),检测波长220 nm,柱温25℃,进样量为20μl。此方法对11种低分子量有机酸的检测限在20~825 ng ml~(-1)之间,回收率在85.57%~100.20%之间,相对标准偏差在0.17%~5.84%之间。实际土壤样品分析结果表明,该方法能够满足土壤低分子量有机酸的痕量检测要求。  相似文献   

2.
反相HPLC法快速测定鸭蛋蛋黄粉中胆固醇含量   总被引：2，自引：0，他引：2  
通过RP-HPLC方法，比较了不同的流动相、流速、检测波长和温度对鸭蛋蛋黄粉中胆固醇分离效果的影响。确定试验最佳条件为：流动相：乙睛：甲醇：异丙醇＝50∶80∶10(体积比)，柱温45℃，进样量20 μL，流速1.3 mL/min，检测波长205 nm。在此条件下测得的天然红心鸭蛋蛋黄粉和普通鸭蛋蛋黄粉中胆固醇的含量分别为24.84 mg/g和25.75 mg/g。  相似文献   

3.
建立一种快速测定豆芽中4-氯苯氧乙酸钠残留量的高效液相色谱法。以市售的豆芽作为供试样品,用酸性氯化钠溶液提取,经乙醚萃取净化,氮吹浓缩。采用Waters Symmetry Shield C18色谱柱(4.6 mm×250 mm,5μm),以甲醇和0.01 mol/L磷酸盐缓冲液(35∶75)为流动相,色谱检测波长为228 nm,并用二极管阵列检测器记录色谱峰的紫外吸收光谱。结果表明,该方法标准曲线线性关系良好,线性范围为0.20~4.00μg/m L,相关系数0.9997;加标回收率在87.6%~95.2%,最低检出限为0.02 mg/kg。该方法操作简便、快捷、准确可靠。  相似文献   

4.
砂质潮土中五种磺胺类药物的高效液相色谱检测方法   总被引：2，自引：0，他引：2  
建立了固相萃取-高效液相色谱法(SPE-HPLC)测定砂质潮土中磺胺嘧啶、磺胺甲基嘧啶、磺胺甲氧嗪、磺胺-5-甲氧嘧啶、磺胺甲恶唑5种磺胺类药物残留的方法。优化后的色谱条件为:流动相比例为磷酸缓冲液(pH=2.3)∶乙睛=80∶20(V/V),流速1.0 mL/min,检测波长270 nm,柱温35℃,进样体积20μL。在优化条件下,5种磺胺类药物的最低检测限在2.4~4.9μg/kg之间,方法的线性范围为0.2~20 mg/kg,线性相关系数均达到0.999 9。砂质潮土中,在添加浓度为0.5、1.5 mg/kg磺胺类药物时平均回收率范围为70.03%~89.65%,相对标准偏差≤10%,能够满足实际样品的分析要求。  相似文献   

5.
蝴蝶兰类原球茎DNA总甲基化水平测定方法的研究   总被引：1，自引：1，他引：0  
刘福平  陈淳  张文惠 《核农学报》2010,24(4):752-756
探讨DNA提取中不同蛋白质变性剂对胞嘧啶(C)和5-甲基胞嘧啶(5mC)色谱的影响,建立蝴蝶兰类原球茎DNA总甲基化水平的HPLC测定方法。本实验采用2种CTAB法(蛋白质变性剂不含酚和含酚)提取基因组DNA,水解后分别以反相HPLC测定C和5mC含量。色谱条件为:色谱柱HypersilBDS Cl8,甲醇-10mmol/L戊烷磺酸钠-三乙胺(6∶90∶0.2,V/V)为流动相,流速0.5ml/min,检测波长273nm。应用不含酚变性剂所提取DNA的水解液C和5mC能较有效分离。以本试验优化的DNA提取方法和HPLC色谱条件,基因组DNA水解液的C和5mC色谱可得到较好的效果。  相似文献   

6.
本文介绍了用高效液相色谱测定配合饲料添加剂中喹乙醇含量的方法。该方法色谱条件为:μ-Bondapak C_(18)色谱柱,甲醇/水(60/40,V/V)作流动相,流速为1.0mL/min;高灵敏可变紫外检测器,检测波长为262nm.标准曲线的线性范围在0～1mg.平均回收率为98.33%。变异系数为3.88%.该方法简便、快速,灵敏、准确。  相似文献   

7.
建立了高效液相色谱法测定饲料中吡啶甲酸铬的方法。样品用乙腈提取,采用C18反相色谱柱,以磷酸盐缓冲液︰乙腈为流动相梯度洗脱, 264 nm检测。吡啶甲酸铬在0.1～20μg/m L浓度范围内线性关系良好,相关系数r~2=1,添加浓度为0.49～99.3 mg/kg,平均回收率为72.0%～101%, RSD为1.2%～8.9%。配合饲料、浓缩料的检出限为0.2 mg/kg,定量限为0.5 mg/kg;预混料检出限为0.5 mg/kg,定量限为1 mg/kg。结果表明,该方法简便、准确,可作为饲料中吡啶甲酸铬的质量控制方法  相似文献   

8.
为有效测定土壤中土霉素残留量,建立了固相萃取－高效液相色谱法提取以及测定潮土、红壤、紫色土中土霉素残留量的方法。土壤中土霉素残留经提取缓冲溶液进行有效提取,经过DVB固相萃取小柱纯化、无水甲醇洗脱和氮气流浓缩后,经HPLC测定。对提取缓冲液、流动相以及流动相pH值、有机相与无机相的比例以及流速等测定条件进行优化研究。结果表明：提取液为Na2EDTA-Mcllvaine,流动相为乙腈∶0.01mol/L磷酸二氢钠（pH值2.5,V∶V=10∶90）,温度25℃,流速1.2ml/min,检测波长350nm对3种不同性质的土壤中土霉素残留量的测定最为合适。应用本方法进行土壤中土霉素残留量的测定,土霉素含量与峰面积具有良好的线性关系,相关系数（n=9）分别为红壤0.997,紫色土0.995,潮土0.987;检出限分别为红壤0.11mg/kg,紫色土0.17mg/kg,潮土0.09mg/kg;回收率(n=18)分别为红壤80.7%~128.8%,紫色土70.5%~100.0%,潮土61.5%~103.9%;相对标准偏差(RSD, n=18)分别为红壤7.1%~28.2%,紫色土11.9%~38.1%,潮土4.1%~17.0％。本方法简便、准确,适合于测定不同土壤中土霉素残留量,结果可靠。  相似文献   

9.
目的:建立茶汤内含物质儿茶素和生物碱检测方法体系,为研究茶汤滋味物质做基础。方法:以X-select-T3(4.6 mm×250 mm,5μm,美国waters)为色谱柱,流动相A:2%甲酸;流动相B:甲醇;甲醇洗脱方式:0 min(83%A,17%B)-9 min(73%A,27%B)-15 min(58%A,42%B)-18 min(83%A,17%B),检测波长275 nm,流速1 m L·min~(-1),柱温30℃。利用保留时间和光谱图定性,外标法定量,分析茶汤滋味物质儿茶素组分和生物碱类物质。结果:儿茶素组分和生物碱回归方程相关性系数都在0.999 0以上,有良好的线性关系,各组分加样回收率为103.68%~82.94%,RSD为0.23%~3.31%。结论:该方法操作简单、快速、准确,可用于茶汤滋味物质儿茶素组分及生物碱的含量测定。  相似文献   

10.
实验建立了离子色谱技术同时测定南瓜中Cr(Ⅲ)和Cr(Ⅵ)的方法。南瓜样品中的Cr(Ⅲ)经过柱前衍生为2,6-嘧啶二羧酸铬,柱后衍生为1,5-二苯碳酰二肼铬,分别于365 nm和530 nm的波长下检测。实验将淋洗液p H控制在6.5~6.8之间,且调节I–的浓度为5 mmol/L。通过制定柱前衍生的水浴加热温度、加热时间和柱后衍生液流速的3因素4水平[L16(43)]正交设计试验,结合各因素水平影响的情况下峰面积变化趋势,最终选取0.5 m L/min为柱后衍生液的流速;而柱前衍生采用100℃为最佳水浴温度,5 min为最佳加热时间。优化了离子色谱条件,提高了检测的灵敏度,Cr(Ⅲ)和Cr(Ⅵ)的方法检出限分别为0.17 mg/kg和0.019 mg/kg。南瓜样品中Cr(Ⅲ)的加标回收率为82%~85%。采用该离子色谱法测定南瓜中的Cr(Ⅲ)和Cr(Ⅵ),结果表明Cr(Ⅵ)未检出。  相似文献   

11.
A novel method has been developed to determine As-containing animal feed additives including roxarsone (ROX), p-arsanilic acid (p-ASA) and nitarsone (NIT), as well as other organic As species (dimethylarsonic acid (DMAA) and monomethylarsonic acid (MMAA)) by ion-pairing high-performance liquid chromatography coupled to hydride generation atomic fluorescence spectrometry (IP-HPLC-HG-AFS). A simple isocratic reversed-phase (RP) HPLC method with a mobile phase containing citric acid and sodium hexanesulfonate (pH 2.0) was developed using a C(18) column. The use of an organic solvent free mobile phase turns this methodology into an environmentally friendly alternative. Several ion pair forming agents, such as sodium hexanesulfonate, tetrabutylammonium bisulfate and perfluoroheptanoic acid, were studied. The limits of detection for As species were calculated in standard solution and resulted to be 0.2, 0.5, 0.6, 1.6, and 1.6 μg As L(-1) for MMAA, DMAA, p-ASA, ROX and NIT, respectively. This method exhibited convenient operation, high sensitivity and good repeatability. It was applied to As speciation in different samples including arugula, dog food, dog urine and chicken liver.  相似文献   

12.
A method for the comprehensive analysis of hydrophilic metabolites, based on a combination of high-performance liquid chromatography and mass spectrometry, is described. We evaluated three types of stationary phases to achieve the separation of highly hydrophilic metabolites. Good chromatographic retention and separation of these metabolites were achieved on a pentafluorophenylpropyl-bonded silica column with gradient elution, using 0.1% aqueous formic acid and acetonitrile as the mobile phase. The optimized conditions allowed the comprehensive determination of the standard 49 kinds of amino acids, 6 kinds of amines, 45 kinds of organic acids, 18 kinds of nucleic bases, 5 kinds of nucleosides, and 14 kinds of nucleotides, and then the linearity, dynamic range, detection limit, and precision of the retention time and the peak area were validated. We applied this method for the targeted analysis of the components in soy sauce. The results from the quantitative determination of amino acids were compared to those obtained with an amino acid analyzer, and the accuracy was in the range between 85 and 119%. The accuracy of other detected components was confirmed to be 105-133% by the recovery rate after the addition of standard compounds. We also applied the method for the nontargeted metabolic profiling of the components in several kinds of soy sauces with the principal component analysis. They were classified by the manufacturing methods, and the components that corresponded to the differences were identified. This method could be useful for the targeted analysis of hydrophilic metabolites as well as their nontargeted metabolic profiling.  相似文献   

13.
A synchronous derivative spectrofluorometric method is described for the determination of the plant growth regulator, gibberellic acid (GA3). The method is based on the formation of a fluorogen in concentrated sulfuric acid. The reaction is carried out at 85% sulfuric acid and in aqueous medium. The common fluorometric method with a linear dynamic range of 137-400 ppb, and a detection limit of 48 ppb is described. The synchronous first and second derivative method has linear dynamic ranges between 7.6-40 ppb and 12-40 ppb, with detection limits of 3.5 and 6.7 ppb, respectively. The influence of reaction variables and of other plant growth regulators present, and the application to residues on oranges, lemons, and grapes, are also described.  相似文献   

14.
牛粪水酸化贮存过程中氮形态转化的特性研究   总被引：3，自引：1，他引：3  
近年来,随着畜禽养殖规模化的快速发展,养殖粪水的处理和利用已成为养殖业健康发展的难点和热点,粪水酸化技术是通过向粪水中添加酸化剂以降低氨气排放,减少粪水贮存中氮素损失的技术,目前此技术已经在丹麦等国推广应用,但中国对此技术的研究尚未起步,为探究粪水酸化固持氮素的效果,该研究以硫酸和明矾为粪水酸化剂,以固液分离前后奶牛粪水为处理对象,通过向粪水中添加酸化剂降低粪水pH值至6.0,分析粪水贮存中氨气排放、氮素转化以及粪大肠菌群数等指标,探索粪水酸化贮存过程氮形态转化机理。研究表明:向养殖粪水中添加酸化剂可降低6.3%~11.1%的总氮损失,能够降低粪水贮存初期中氨气的排放,同时有效抑制了奶牛粪水中粪大肠菌群的活性,使其更易达到无害化处理。酸化剂的加入一方面抑制粪水中微生物作用下的有机氮向无机氮素的转化,提高粪水贮存中有机氮的含量,减少铵态氮的产生量,另一方面酸化剂与粪水中的铵态氮结合生成稳定的铵盐,抑制了粪水中铵态氮向氨气转化的化学平衡,降低了粪水中因氨气排放导致的总氮损失,从而达到减少粪水贮存中氮素损失。  相似文献   

15.
Two analytical methodologies for the simultaneous analysis of eight sulfonamide antibiotics in animal feeds were developed. Analytes were extracted in a simple and rapid procedure by manual shaking with an ethyl acetate/ultrapure water mixture (99:1, v/v) without further sample cleanup. Mean recoveries ranging from 72.7% to 99.4% with relative standard deviations below 9% were achieved from spiked animal feed samples. Determination was carried out by high-performance liquid chromatography using fluorometric detection with precolumn derivatization. The separation of the derivatized compounds was performed using two different chromatographic columns: a conventional C(18) column and a recently available core-shell particle Kinetex C(18) column. Both methods were validated in-house in six different feed matrices, and the two approaches were compared. The experiments showed that the method using the Kinetex column was superior with regard to speed of analysis and precision, both under repeatability and intermediate reproducibility conditions. The limits of detection and quantification were also greatly improved, below 0.10 and 0.34 μg/g, respectively. Finally, this novel approach was successfully applied to the analysis of real feed samples.  相似文献   

16.
Soil macroinvertebrates are highly diverse and their major ecological service include breakdown of organic matter and in turn improve soil fertility and pill-millipedes are well-known for their significant role in ingestion, disintegration and decomposition of organic matter in soil. This study characterized the feed, the decomposing leaf litter of coconut (Cocos nucifera), and faeces of two endemic giant pill-millipedes Arthrosphaera disticta and A. fumosa collected from forests of the Western Ghats of India based on chemical features and microbial profile. In both millipedes, electric conductivity and total phosphorus were significantly increased in faeces, while the crude protein, organic carbon, total nitrogen and total phenolics were significantly decreased,as compared to those in feed. Heterotrophic bacteria, actinomycetes, rhizobia and phosphate-solubilizing bacteria were significantly higher in faeces than in feed, while filamentous fungi and yeast substantially decreased in faces compared to feed in both the millipedes. Spectrum of fatty acid methyl esters was considerably different between feed and faeces of both the millipedes. The total saturated fatty acids were higher than the total unsaturated fatty acids in feed as well as faeces, while the ratio of unsaturated/saturated fatty acids decreased from feed to faeces. Dodecanoic and tetradecanoic acids in A. disticta and octadecanoic acid in A. fumosa significantly increased, while (9Z)-octadec-9-enoic and (9E,12E)-octadeca-9,12-dienoic acids in A. disticta and hexadecanoic, tetracosanoic and (9E,12E)-octadeca-9,12-dienoic acids in A. fumosa significantly decreased in faeces compared to feed, indicating millipede-dependent changes in fatty acids. Icosanoic acid was present in faeces of both the millipedes, and hexadec-9-enoic acid was confined to faeces of A. disticta, while pentadecanoic, heneicosanoic, (9Z,12Z,15Z)-9,12,15-octadecatrienoic and eicosenoic acids were confined to faeces of A. fumosa. Pill-millipedes enrich the soil quality by leaf litter conditioning in their gut through specific microbial communities. Fingerprinting of fatty acid methyl esters in faeces of these millipedes reflected the activity of specific microbial population in their guts.  相似文献   

17.
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.  相似文献   

18.
A modified liquid chromatographic method is described for the determination of Gentian Violet (GV) in animal feed. The reliable detection limit is 0.5 ng (reference standards), and 1 ppm GV was reliably determined in feed. The calibration curve was linear between 1 and 40 micrograms/mL. The method, developed in a study by the National Center for Toxicological Research, was modified to use methanol-water (9 + 1) instead of benzene-methanol as the eluting solution in the column cleanup. GV is extracted from feed with methanol-1N HCl (99 + 1), cleaned up on a Sephadex LH-20 column to remove any remaining interferences, separated on a Nova-Pak C18 column fitted with a precolumn filter, and determined at 588 nm. The identity of GV is confirmed by thin-layer chromatography (Rf = 0.47) by comparison with a reference standard. Average recoveries from 3 sets of 5 feed samples containing 2.5, 5.0, and 10.0 ppm GV were 115, 95, and 102%, respectively.  相似文献   

19.
畜禽养殖粪水酸化贮存及氮素减损增效研究进展   总被引：1，自引：0，他引：1  
畜禽粪水酸化贮存能够有效调控粪水贮存中微生物、环境与氮素间的作用关系,实现粪水氮素的减损增效,是一种具有广泛应用前景的关键技术。该研究系统综述了粪水酸化贮存中氮素的迁移转化机理,比较评价了常见酸化剂和不同酸化贮存工艺的应用效果,分析了酸化贮存技术对粪水氮素减损增效的影响。梳理总结得到,粪水酸化存储中氮素的迁移转化机制主要包括有机氮矿化、铵态氮固持、无机氮转化的抑制及硝化3个关键环节,可以依靠改变微生物作用和化学平衡状态实现氮素的减损;与其他酸化工艺相比,长期酸化工艺具有酸化效果更加稳定、应用范围较为广泛等优势;粪水酸化技术能够大幅降低NH3排放,以及部分N2O的排放,进而提高粪肥还田后土壤肥效,但不合理的酸化贮存技术及施用方式也会降低粪水肥效,甚至引起二次污染;未来应重点从氮素迁移转化路径的定量分析、复合酸化剂的开发、粪肥施用效果及风险的评估应对等方面进行深入研究。  相似文献   

20.
A high-performance liquid chromatographic (HPLC) method with diode-array detection (DAD) was used to identify and quantify free and total phenolic acids (m-hydroxybenzoic acid, p-hydroxybenzoic acid, protocatechuic acid, gallic acid, vanillic acid, syringic acid, o-coumaric acid, m-coumaric acid, p-coumaric acid, caffeic acid, ferulic acid, sinapic acid, chlorogenic acid, and ellagic acid) in plant foods. Free phenolic acids were extracted with a mixture of methanol and 10% acetic acid. Bound phenolic acids were liberated using first alkaline and then acid hydrolysis followed by extraction with diethyl ether/ethyl acetate (1:1). All fractions were quantified separately by HPLC. After HPLC quantification, results of alkali and acid hydrolysates were calculated to represent total phenolic acids. Ellagic acid was quantified separately after long (20 h) acid hydrolysis. The methods developed were effective for the determination of phenolic acids in plant foods. DAD response was linear for all phenolic acids within the ranges evaluated, with correlation coefficients exceeding 0.999. Coefficients of variation for 4-8 sample replicates were consistently below 10%. Recovery tests of phenolic acids were performed for every hydrolysis condition using several samples. Recoveries were generally good (mean >90%) with the exceptions of gallic acid and, in some cases, caffeic acid samples.  相似文献   

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