Development of an efficient extraction method for oxytetracycline in animal manure for high performance liquid chromatography analysis

Oxytetracycline (2-(amino-hydroxy-methylidene)-4-dimethylamino-5,6,10,11,12a-pentahydroxy-6-methyl-4,4a,5,5a-tetrahydrotetracene-1,3,12-trione) is a major member of the tetracycline antibiotics family of which are widely administered to animals in concentrated animal feeding operations for purposes of therapeutical treatment and health protection. With the disposal of animal manure as fertilizer into agricultural land, tetracyclines enter the environment. However, tetracyclines chelate with multivalent cations and proteins, resulting in low extraction efficiencies from animal manure for tetracycline residue analysis. In this study an efficient extraction method for oxytetracycline from steer manure using methanol/water solution amended with chelating organic acid was developed for the analysis of high performance liquid chromatography. The effect of species and amount of amendment acids, shaking time, methanol/water ratio, manure weight, and repeated times of extraction was investigated. It was optimized to amend 2.5 g citric acid and 1.1 g oxalic acid with 10.0 g manure sample in a 50-ml centrifuge tube and extract with 15 ml methanol/water (9:1 in volume) by vigorously shaking for 30 min in a reciprocating shaker. After centrifugation at 11,000 rpm, supernatant is collected. Sample was extracted for a total of 3 times. The developed extraction method was further applied to extract oxytetracycline from fresh and aged cow manure, swine and poultry manure, and soil. Satisfactory recoveries ranging from (84.1 ± 2.4) % to (102.0 ± 3.1) % were obtained, demonstrating that the optimized extraction method is robust for oxytetracycline from different manure sample matrixes.     

Determination of aromatic hydrocarbons in submicrogram quantities in aqueous systems by means of high performance liquid chromatography

One liter of the water sample is extracted with 1,1,2-trichlorotrifluoroethane. This non-polar solvent with a low boiling point is then concentrated and a portion of the concentrated extract is injected in a high performance liquid chromatography system. Polar material is separated from the hydrocarbons by means of a silica gel column. The detector measures the UV absorbance at 254 nm at which wavelength aromatic compounds absorb especially well. The quantitative values are given as phenanthrene equivalents and amounts as small as 20 ng/l can be detected. The standard deviation of the method is ± 50 ng/l. Both these values can be improved with a limited amount of difficulty. A concentrated sample extract can be injected and evaluated in less than 6 minutes, and the method is simple enough to have been used at sea.     

反相高效液相色谱法测定污水中壬基酚聚氧乙烯醚总量

建立了固相萃取一反相液相色谱一荧光检测法分析污水中壬基酚聚氧乙烯醚总量的方法.固相萃取采用Wa-ters Oasis HLB固相萃取柱(30 μg×60 mg×3 mL),6 mL二氯甲烷/甲醇(90/10,V/V)混合溶剂洗脱,洗脱液用氮吹仪浓缩至1 mL,回收率为99.68%.采用ZORBAX Eclipse XDBC-18(4.6 mm×150 mm,5 μm)反相色谱柱,甲醇/水为流动相,流速1.0 mL/min,以每分钟增加2.5%的梯度陡度进行洗脱,流动相中甲醇比例由70%增加到100%,柱温23℃,进样量15μL.荧光检测器的激发波长230 nm,发射波长313 nm.采用外标法定量.该方法的空白加标和污水样品加标回收率均在90%以上,标准偏差小于10%,定量下限为0.97～1.90 μg/L.利用该方法分别对污水处理厂进水水样、二级处理出水水样、再生水水样进行了测定,测定结果的准确度和精密度满足痕量分析的要求.     

Estimating the aqueous solubility of aromatic hydrocarbons by high performance liquid chromatography

Empirical equations which correlate high performance liquid chromatography capacity factor (k′) to aromatic hydrocarbon aqueous solubility are developed. The correlations of k′ to octanol-water partition coefficients, and k′ to hydrocarbon surface area are also shown.     

Variation in estrogenic activity among fractions of a commercial nonylphenol by high performance liquid chromatography

Estrogenic activity by recombinant yeast screen assay of the commercial NP was considerably higher when compared with that of n-nonylphenol (n-NP). Fractionation of the commercial NP by high performance liquid chromatography (HPLC) afforded seven isomers: 4-(1,3-dimethyl-1-propyl-butyl)-phenol, 4-(1,1,3-trimethyl-hexyl)-phenol, 4-(1,1-dimethyl-3-ethyl-pentyl)-phenol, 4-(1,1,4-trimethyl-hexyl)-phenol, 4-(1-methyl-1-propyl-pentyl)-phenol, 4-(1,1,2-trimethyl-hexyl)-phenol and 4-(1-ethyl-1-methyl-hexyl)-phenol. The structures of these isomers were determined by GC-MS and nuclear magnetic resonance spectroscopy (NMR). All of these isomers possessed tertiary alpha-carbon in their chemical structures. Another tertiary NP, 4-(1,1-dimethyl-heptyl)-phenol was synthesized in the present study and this synthetic NP also exhibited the estrogenic activity. One fractionated compound was identified as one of decylphenol, 4-(1-ethyl-1,4,4-trimethyl-pentyl)-phenol. The isomer, 4-(1,1,4-trimethyl-hexyl)-phenol exhibited the highest estrogenic activity corresponding to 1/10000 that of 17beta-estradiol (E2). The activity of n-NP was the least. This suggests that it may be possible to develop a technical NP mixture with relatively low estrogenic activity.     

Monitoring transport of selected pesticides and phenols in soil columns by high performance liquid chromatography

Abstract

Soil columns were used to study pesticides and phenols transport under rapid infiltration land treatment conditions. An analytical procedure is described for the quantitative determination of atrazine, diuron, carbofuran, phenol, 2,4‐dinitrophenol, 2,4‐dimethylphenol, and 2,4‐dichlorophenol in soil and wastewater. Recoveries of all analytes were greater than 90%. The method detection limits for all analytes were ≤0.03 μg/ml (s/n=4) in wastewater and ≤ 0.1 μg/ml (s/n=5) in soil.     

Speciation of arsenic and chromium metal ions by reversed phase high performance liquid chromatography

The speciation of arsenic [As(III) and As(V)] and chromium [Cr(III) and Cr(VI)] was carried out by high performance liquid chromatography. The column used was Econosil C18 (250 x 4.6 mm i.d., particle size 10 microm). The mobile phases consisted of water-acetonitrile (80:20, v/v) for arsenic and 10 mM ammonium acetate buffer (6.0 pH)-acetonitrile (10:90, v/v) for chromium speciation separately and respectively. The detection was carried out by UV-Vis at 410 nm and atomic absorption spectrometer (AAS) respectively and separately. The values of alpha and Rs of As(III) and As(V) species were 1.4 and 1.5 respectively while the values of alpha and Rs for Cr(III) and Cr(VI) were 1.35 and 0.2 respectively. The effect of the acetonitrile percentages was also carried out on the speciation of arsenic only. The relative standard deviation and limit of detection were in the range of 0.01-0.02 and 0.4-1.0 microg/ml respectively.     

高效液相色谱法检测水中5种微囊藻毒素

使用Agilent1260型高效液相色谱仪,建立定量测定天然水体中5种微囊藻毒素（MC-RR、YR、LR、LA、LY）的分析方法。比较甲醇/三氟乙酸（TFA）水溶液与甲醇/磷酸两种流动相体系,待测物质的响应程度,结果发现,TFA作为缓冲溶液时,基线较磷酸稳定,因此,选择甲醇/TFA水溶液作为流动相。比较不同TFA体积比例,待测物质的分离程度,结果显示,甲醇/0.02%的TFA水溶液作为流动相时,5种MCs含量的分离度较好。比较等度和梯度洗脱条件,发现,梯度洗脱条件5种MCs的分离度较等度洗脱条件好。该方法 MC-RR、YR、LR、LA、LY的最低检出限（LOD）分别为0.015、0.035、0.018、0.032和0.026μg/L,最低定量限（LOQ）分别是0.049、0.117、0.062、0.106和0.086μg/L。在0.10～1.50μg/mL的线性范围内,相关系数R2≥0.99,实际水样回收率为73.9%～103.3%。     

A high performance liquid chromatography method for determination of gas-phase hydrogen peroxide in ambient air using Fenton's chemistry

A new method for determination of hydrogen peroxide in atmospheric samples is described. Cryogenically collected H2O2 is reacted with sodium salicylate in the presence of Fe(2+) to produce dihydroxybenzoate, which is separated from the reaction mixture by high performance liquid chromatography and detected by UV absorption. Measurements of atmospheric H2O2 were conducted in Las Vegas, NV from June 1999 to December 1999 to evaluate and characterize the method. Measured mixing ratios of H2O2 (there were also non-detects) ranged from 0.012 to 2.74 ppbv, with expected correlations to primary gaseous pollutants and strong seasonal variation consistent with a photochemically derived species. It was concluded that the method is easy to use and has sufficient sensitivity and selectivity to be useful in atmospheric monitoring.     

紫外—荧光检测器高效液相色谱法测定PM2.5中16种多环芳烃

建立了一种利用高效液相色谱(HPLC)同时分离和测定大气颗粒物中16种优控多环芳烃(PAHs)的方法。样品经二氯甲烷超声提取,浓缩后经乙腈定容,以乙腈和水作为流动相进行反相HPLC梯度淋洗分离后,由紫外检测器串联程序波长荧光检测器检测。通过实验条件的优化,实现了16种PAHs组分基线完全分离和高灵敏度检测。16种PAHs检测限为0.05～1.20μg/L,回收率在75.0%～106.0%,相对标准偏差在0.27%～7.42%,均符合方法学的要求。将该方法用于测定贵阳市不同功能区PM2.5中PAHs的含量,具有快速简便、准确灵敏、重现性好等优点,适合大批量样品的分析。     

Aqueous solubility of polychlorinated dibenzo-p-dioxins determined by high pressure liquid chromatography

Water solubilities (S_W) determined by the HPLC generator column method are reported for a series of chlorinated dibenzo-$\text{p}$-dioxins (PCDDs) with S_W ranging from 0.4 ng/L (ppt) for octa-chlorodibenzo-$\text{p}$-dioxin to 430 ng/L for 1,2,3,7-tetrachlorodibenzo-$\text{p}$-dioxin at 20°C. A correlation is demonstrated between S_W and HPLC capacity factors (k′) for these extremely hydrophobic compounds, allowing calculation of S_W of PCDDs from k′ and melting point data.     

A simple procedure for determining octanol-water patition coefficients using reverse phase high performance liquid chromatography (RPHPLC)

The logarithm of the capacity factor of several organic compounds determined by reversed-phase high performance liquid chromatography on a commercially available C₁₈ column is shown to be linearly related to the logarithm of the n-octanol/water partition coefficient. Calculated values for test compounds show good agreement with literature values.     

环境水体中四溴双酚A的HPLC-MS/MS分析方法的建立与应用

四溴双酚A(tetrabromobisphenol A,TBBPA)是目前使用量最大的溴代阻燃剂.随着它的广泛应用,已经引起了大气、水体、沉积物和土壤等环境介质及相关生态系统的严重污染.建立了环境水体中TBBPA的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法.该方法采用电喷雾电离(ESI)负离子模式进行扫描,...     

Effect of liquid manure on the mole fraction of nitrous oxide evolved from soil containing nitrate

The same emission factor is applied to fertiliser N and manure N when calculating national N2O inventories. Manures and fertilisers are often applied together to meet the N needs of the crop, but little is known about potential interactions leading to an increase in denitrification rate or a change in the composition of the end-products of denitrification. We used the 15N gas-flux method in a laboratory experiment to quantify the effect of liquid manure (LM) application on the fluxes of N2 and N2O when the soil contained fertiliser 15NO3-. LM increased the mole fraction of N2O from 0.5 to 0.85 in the first 12 h after application. More than 94% of the N2O was from the reduction of NO3-, probably due to aerobic nitrate respiration as well as respiratory denitrification.     

Determination and identification of polycyclic aromatic hydrocarbons in smoked and charcoal-broiled food products by high pressure liquid chromatography and gas chromatography.

A high pressure liquid chromatographic procedure has been developed and applied to the analysis of polycyclic aromatic hydrocarbons (PAH's) in 70 samples of smoked food products commercially available in Canada, and in 6 charcoal broiled meats. In some cases a gas-liquid chromatographic procedure was used as a confirmatory technique. In the commercial samples PAH's were detected in approx. 70% of the samples. Total PAH's ranged from 0-141 ppb and individual PAH's from 0-38 ppb. With the charcoal-broiled samples, total PAH's and individual PAH's ranged from 0-164 ppb and 0-60 ppb respectively. These levels are similar to those observed in other countries.     

Reverse phase high performance liquid chromatographic determination of Baygon in water

Abstract

A simple analytical procedure for determination of Baygon in water is described. The Baygon residues are extracted on a C₁₈ SEP‐PAK cartridge and subsequently analyzed by reverse phase high performance liquid chromatography using ultraviolet detection at 272 nm. Water samples spiked with Baygon are found to give greater than 90 percent recoveries.

Concentration levels as low as 20 ppb can be easily detected by this method.     

Reverse phase high performance liquid chromatographic determination of Baygon in water

A simple analytical procedure for determination of Baygon in water is described. The Baygon residues are extracted on a C18 SEP-PAK cartridge and subsequently analyzed by reverse phase high performance liquid chromatography using ultraviolet detection at 272 nm. Water samples spiked with Baygon are found to give greater than 90 percent recoveries. Concentration levels as low as 20 ppb can be easily detected by this method.     

Sun light degradation of 4-chloroaniline in waters and its effect on toxicity. A high performance liquid chromatography - Diode array - Tandem mass spectrometry study

This paper studies the degradation reactions that 4-chloroaniline can naturally undergo in waters for the action of sun light. 10.00 mg L⁻¹ 4-chloroaniline aqueous solution, without any addition of organic solvent, are undergone to photoirradiation under conditions that simulate sun light. The degradation pathway, followed by HPLC-DAD-MS/MS methods, is complex since the pollutant gives rise to many photoproducts: the predominant species are characterized by m/z values of 217 (P5) and 218 (P6) and are compatible with dimeric structures of 4-chloroaniline. Vibrio fischeri tests indicate that the photoproducts of 4-chloroaniline are characterized by a toxicity level significantly greater than the precursor.     

SBR处理高浓度养猪废水工艺条件

以养猪场废水作为研究对象,采用序列间歇式活性污泥法SBR,通过实验研究了供气量、pH、排泥量、原水稀释倍数、水力停留时间（HRT）对SBR出水水质的影响。结果表明,供气量为375 L/（min·m³）、pH为8.0,并添加排泥100 mL的操作,可使SBR处理效果明显提高,COD、磷和凯氏氮去除率最高分别可达96.37%、94.14%、99.38%。逐步降低进水稀释倍数有利于培养出处理高浓度有机养猪废水的活性污泥,可将平均COD、磷和凯氏氮含量高达9 161.24、33.41和1 502.77 mg/L的养猪废水处理至出水的490.11、5.35和17.84 mg/L。降低HRT对SBR去除率影响不大。