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1.
土壤及畜禽粪肥中四环素类抗生素固相萃取-高效液相色谱法的优化与初步应用 总被引：5，自引：0，他引：5
本研究优化了土壤和有机肥中3 种四环素类抗生素的提取和测定方法。方法经优化后,土壤和有机肥中的抗生素的提取效率达到52%~95%,且分析时间大大缩短。本研究还利用优化方法在天津进行了有机肥和菜地中3 种抗生素残留的初步调查。集约化养殖场的猪、鸡粪便中四环素类抗生素残留状况为: 金霉素（CTC）检出率达到78%,最高残留值达到563.8 mg/kg（干基）; 四环素（TC）和土霉素（OTC）检出率也高达56%,最高值分别达到34.8 mg/kg 和 22.7 mg/kg。在天津销售的几种商品有机肥中同样检测出四环素类抗生素的残留,残留水平与猪粪和鸡粪相当。菜田土壤样品中TCs的总检出率为64%,3.种抗生素中土霉素检出率最低为18%,最高值达到105.6 g/kg（风干基）; 四环素检出率为36%,最高值达到196.7 g/kg; 金霉素检出率为32%,最高值达到477.8 g/kg。在所调查土壤中,温室和大棚土壤TCs的残留水平高于露地土壤。占调查样品 27.3% 的菜田土壤中TCs总量超过欧盟规定的生态安全触发线（100 g/kg）,存在一定的潜在生态风险。 相似文献
2.
E E Martinez W Shimoda 《Journal of the Association of Official Analytical Chemists》1988,71(3):477-480
A liquid chromatographic method for the multiresidue determination of tetracyclines (TCs) in feeds is described. The levels of quantitation were 10 ppm each for tetracycline-HCl (TC), oxytetracycline (OTC), and chlortetracycline-HCl (CTC); the detection limit was 40 ppb for each. The calibration curves were linear between 2.5 and 100 ppm. The procedure involved double extraction with pH 2.0 and pH 4.5 McIlvain buffers, cleanup on a Sephadex LH-20 column, separation on a Nova-Pak C18 column, and detection at 370 nm. Recoveries of 10 micrograms/g of each TC in multiresidue feed samples ranged from 55.8 to 75.5% for OTC, 71.6 to 100% for TC, and 22.4 to 60.6% for CTC. The identities of the TCs were confirmed by thin layer chromatography. 相似文献
3.
我国有机肥原料及商品有机肥中四环素类抗生素的检出率及含量 总被引：1，自引：0，他引：1
4.
壤和堆肥中四环素类抗生素的检测方法优化及其在土壤中的降解研究 总被引：2，自引：0，他引：2
在对土霉素（OTC）、四环素（TC）和金霉素（CTC）3 种四环素类抗生素的高效液相色谱（HPLC）检测分析方法以及在土壤和堆肥中的提取方法进行改进和优化的基础上,采用该方法进行了 3 种抗生素在土壤中的降解试验。结果表明,选用 Agilent Eclipse XDB-C8（4.6150 mm,5 m）色谱柱,以 0.01 mol/L草酸/乙腈/甲醇（79/10.5/10.5,v/v/v）为流动相,紫外检测波长 268 nm,流速 1.0 mL/min,进样量 5 L,采用外标法定量,可使 3 种四环素类抗生素在 20 min 内全部洗脱并达到基线分离; 在 0~10 mg/L 范围内,抗生素浓度与峰面积呈显著的线性关系,相关系数（r）均 0.999。土壤和堆肥样品中的 OTC、TC 和 CTC可用1 mol/L NaCl/0.5 mol/L 草酸/乙醇（25/25/50,v/v/v）混合溶液提取,其回收率在 76.0%~92.5% 之间。加入到土壤中的抗生素在 25℃下避光培养 49 d 后,在壤土和红土中的降解率分别是 67%~72% 和 36%~46%,对应的半衰期分别为 2630 d 和 4675 d,说明抗生素在壤土中比红土中容易降解。此外,3种抗生素在壤土中的半衰期没有显著性差异,而在红土中 CTC 和 TC 的降解速率显著高于 OTC。 相似文献
5.
A method was validated for analysis of oxytetracycline (OTC), tetracycline (TC), and chlortetracycline (CTC) in fortified salmon muscle tissue. Recoveries of OTC were 100 +/- 6, 86 +/- 6, and 82 +/- 5% (n = 6) at fortification levels of 1.0, 0.5, and 0.2 ppm, respectively. Recoveries of TC were 68 +/- 4, 65 +/- 6, and 66 +/- 7%; recoveries of CTC were 45 +/- 9, 48 +/- 8, and 0%, respectively. Detection limits for OTC and TC were 0.08 and 0.09 ppm, respectively. 相似文献
6.
Two agricultural soils were collected from Dahu and Pinchen counties and swine manure compost (SMC) from Pingtung County in Taiwan, China to investigate the sorption and dissipation of three tetracyclines (TCs), i.e., oxytetracycline (OTC), tetracycline (TC) and chlortetracycline (CTC), in compost, soils and soil/compost mixtures with different organic carbon (OC) contents. There were seven treatments in total. TCs were most strongly adsorbed to SMC in all treatments due to the high OC content. When SMC was present in the soils, the sorption of TCs was significantly enhanced, which might be attributed to the increased OC content and CEC. The adsorption of TCs showed non-linear adsorption isotherms and fitted well to the Freundlich model. After 49 d of incubation at 25 oC in soils and soil/compost mixtures in the dark, TCs elapsed in all substrates, with the time required for 50% degradation (DT50) between 20 and 41 d, and the time for 90% degradation (DT90) between 68 and 137 d. Soil amended with compost enhanced the stability of TCs and reduced their mobility. The dissipation of TCs in a soil environment was slow, indicating that these compounds might be persistent in soil. 相似文献
7.
H Oka Y Ikai N Kawamura J Hayakawa 《Journal of the Association of Official Analytical Chemists》1991,74(6):894-896
Tissues were collected to survey the actual conditions of tetracycline antibiotics (TCs) residues in slaughtered animals that did not pass inspection at slaughterhouses in Aichi Prefecture, Japan, because of the presence of disease symptoms. Tissues were analyzed by liquid chromatography. Among 271 samples, 49 (18.1%) were positive for oxytetracycline (OTC), 5 (1.8%) for chlortetracycline (CTC), and 5 (1.8%) for doxycycline (DC), respectively. One sample (cattle kidney) was positive for both OTC and DC. However, tetracycline was not detected in any samples. Percentage frequencies of TCs residues were 29.1% (37/127) and 15.2% (22/144) for cattle and hogs, respectively. Kidney samples showed higher incidence of TCs residues and 1.5-7 times higher residual concentrations than liver and miscellaneous samples. 相似文献
8.
A sensitive and specific method is described for the simultaneous determination of oxytetracycline, tetracycline (TC), and chlortetracycline residues in edible swine tissues, by combining liquid chromatography with spectrofluorometric and mass spectrometry detection. The procedure involved a preliminary extraction with EDTA-McIlvaine buffer acidified at pH 4.0, followed by solid-phase extraction cleanup using a polymeric sorbent. The liquid chromatography analysis was performed with spectrofluorometric detection after postcolumn derivatization with magnesium ions. The limits of quantification were 50 microg/kg for muscle and 100 microg/kg for kidney tissues. The recovery values were greater than 77.8% for muscle and 65.1% for kidney. The method has been successfully used for the quantification of tetracyclines in swine tissues samples. The selective liquid chromatography mass spectrometric analysis for confirmation of oxytetracycline in one positive swine muscle sample was made by atmospheric pressure chemical ionization (APCI). The APCI mass spectra of the TCs gave the protonated molecular ion and two typical fragment ions, required for their confirmation in single ion monitoring scan mode in animal tissues. 相似文献
9.
E E Martinez W Shimoda 《Journal of the Association of Official Analytical Chemists》1989,72(5):848-850
A method for studying McIlvain's solution as a factor in epimerization of chlortetracycline in animal feed has been developed. McIlvain's solution (McBuffer) was used previously to extract oxytetracycline (OTC), tetracycline-HCl (TC-HCl), and chlortetracycline-HCl (CTC-HCl) from animal feed because it gave the best recoveries for all 3 tetracyclines; however, the McBuffer solution caused epimerization of CTC-HCl to 4-epi-chlortetracycline (4-epi-CTC). Recovery results were 30-40% lower for CTC than for OTC and TC from the same sample extract. The levels of concentration tested for CTC and 4-epi-CTC were 10 ppm, the detection limits for both were 3 ppb, and the calibration curves were linear between 5 and 80 ppm for both CTC-HCl and 4-epi-CTC. The present study shows that CTC recoveries averaged 35% lower because of epimerization initiated by the use of McBuffer in the extraction procedure. 相似文献
10.
固相萃取-高效液相色谱法测定有机肥中四环素类抗生素药物残留 总被引：6，自引：0，他引：6
建立了固相萃取-高效液相色谱(SPE-HPLC)法测定有机肥中土霉素(OTC)、四环素(TC)和金霉素(CTC)3种四环素类抗生素残留的方法。肥料样品采用甲醇、EDTA和McIlvaine缓冲液的混合液(pH=7.2)为提取液,用强阴离子交换柱(SAX)-亲水亲脂萃取柱(HLB)串联进行纯化和富集。采用甲醇-乙腈-0.01mol/L草酸溶液为流动相,进行HPLC分析。3种抗生素的线性范围为0.10～20 mg/L,OTC、TC和CTC的检测限分别为0.03、0.03和0.05 mg/L。不同添加水平的样品加标回收率为64%～86%,RSD在4.14%～8.16%之间。该方法测定了上海市场上40种肥料,发现部分样品有四环素类抗生素的残留物。 相似文献
11.
Pena A Pelantova N Lino CM Silveira MI Solich P 《Journal of agricultural and food chemistry》2005,53(10):3784-3788
An analytical method for the determination of OTC and TC residues in honey was developed. Sample treatment involves an extraction in EDTA-McIlvaine buffer, followed by a solid-phase cleanup step. With regard to the cleanup procedure, different SPE cartridges were evaluated and the results presented. The method was validated according to the guidelines laid down by the 2002/657/EC European Decision parameters: decision limit (Cc alpha) and detection capability (CC beta) were 20 and 21 microg/Kg and 49 and 50 microg/Kg for OTC and TC, respectively, and recoveries of OTC and TC from spiked samples, at three fortification levels, were higher than 87% for both compounds. The analytical method was applied to 57 honey samples. 相似文献
12.
Zurhelle G Petz M Mueller-Seitz E Siewert E 《Journal of agricultural and food chemistry》2000,48(12):6392-6396
4-epioxytetracycline and N-demethyloxytetracycline, as metabolites of oxytetracycline (OTC), 4-epitetracycline and N-demethyltetracycline, as metabolites of tetracycline (TC), and 4-epichlortetracycline, isochlortetracycline (ICTC), 4-epi-ICTC, and N-demethyl-ICTC, as metabolites of chlortetracycline (CTC), were detected in egg yolk and plasma obtained from feeding studies with either OTC, TC, or CTC. In egg white, only OTC, TC with its 4-epimer, and ICTC with its 4-epimer were detected in substantial concentrations. The ratios of epimerization and N-demethylation in the eggs did not change during the medication period. The samples were analyzed by an automated HPLC system (ASTED) with UV, fluorescence, or MS-MS detection. 相似文献
13.
2009年在江苏省范围内采集27个规模化养殖场排水口和周围环境水体样品53个,用高效液相色谱-三重四极杆质谱对其中的土霉素（OTC）、金霉素（CTC）、四环素（TC）和强力霉素（DOX）等四环素类抗生素污染进行了检测。结果显示,土霉素、金霉素、四环素和强力霉素在水体样品中的检出率分别为60.4%、60.4%、34.0%和17.0%,污染量分别在0.07～72.91、0.10～10.34、0.08～3.67μg·L-1和0.11～39.54μg·L-1之间,检出率以土霉素和四环素最高;猪养殖场中土霉素、四环素和强力霉素的污染量比牛和鸡场的要高,牛场中金霉素和强力霉素的污染量明显低于鸡场;从区域上看,苏南地区受到的污染明显高于苏北。 相似文献
14.
A R Long L C Hsieh M S Malbrough C R Short S A Barker 《Journal of the Association of Official Analytical Chemists》1990,73(3):379-384
A multiresidue method for the isolation and liquid chromatographic determination of oxytetracycline (OTC), tetracycline (TC), and chlortetracycline (CTC) antibiotics in milk is presented. Blank and tetracycline (OTC, TC, and CTC) fortified milk samples (0.5 mL) were blended with octadecylsilyl (C18, 40 microns, 18% load, endcapped, 2 g) derivatized silica packing material containing 0.05 g each of oxalic acid and disodium ethylenediaminetetraacetic. A column made from the C18/milk matrix was first washed with hexane (8 mL), following which the tetracyclines were eluted with ethyl acetate-acetonitrile (1 + 3; v/v). The eluate contained tetracycline analytes that were free from interfering compounds when analyzed by liquid chromatography with UV detection (photodiode array, 365 nm). Correlation coefficients of standards curves for individual tetracycline isolated from fortified samples were linear (from 0.982 +/- 0.009 to 0.996 +/- 0.004) with average percentage recoveries from 63.5 to 93.3 for the concentration range (100, 200, 400, 800, 1600, and 3200 ng/mL) examined. The inter-assay variability ranged from 8.5 +/- 2.4% to 20.7 +/- 13.0% with an intra-assay variability of 1.0-9.3%. 相似文献
15.
猪粪中3种四环素类抗生素在土壤中的动态变化及降解途径 总被引：1，自引：1，他引：0
采用室内模拟培养试验,研究了180 d内不同用量猪粪中3种四环素类抗生素（TCs）（包括四环素TTC,土霉素OTC,金霉素CTC）在土壤中降解的动态变化规律及降解途径。结果表明,猪粪中3种四环素类抗生素进入土壤后含量均呈现前期迅速下降,中后期减缓的规律,但不同种类和用量处理的变化速率和减少幅度有显著差异（P0.05）。180d时,猪粪处理土壤中的降解率为金霉素土霉素四环素,平均半衰期为17.43d、31.32d、49.48d。降解率与猪粪用量呈负相关,同培养时间呈正相关。猪粪中抗生素在土壤中的降解率要高于纯品抗生素,降解率的增加以外源微生物降解为主,外源微生物降解对四环素的作用最好。综上所述,随着培养时间的延长,猪粪中四环素类抗生素在土壤中能随微生物降解等作用而逐渐减少,但短期内仍可能产生环境危害。 相似文献
16.
The microtiter plate system for turbidimetric assay of chlortetracycline (CTC) and oxytetracycline (OTC) levels in feeds uses a 96 well microtiter plate, a multichannel pipette, and an ELISA reader to measure turbidity. Feeds are extracted for both tetracyclines using AOAC extraction systems. For CTC, the range of the standard curve is 0.001-0.005 microgram CTC/mL; for OTC, the range is 0.004-0.016 microgram OTC/mL. Repeatability of CTC assays, as shown by the coefficient of variation (CV), ranged from 0.54 to 5.65% for same-day assays and from 2.01 to 9.39% for assays on different days. For OTC, CVs ranged from 2.69 to 10.01% for same-day assays and 3.24 to 9.08% for different-day assays. Average recoveries for CTC were 108.7% for same-day assays and 106.8% for different-day assays; for OTC, average recoveries were 112.4% and 106.5% for same-day and different-day assays, respectively. 相似文献
17.
Determination of flubendazole and its metabolites in eggs and poultry muscle with liquid chromatography-tandem mass spectrometry 总被引：3，自引：0，他引：3
De Ruyck H Daeseleire E Grijspeerdt K De Ridder H Van Renterghem R Huyghebaert G 《Journal of agricultural and food chemistry》2001,49(2):610-617
The optimization of a quantitative and sensitive LC-MS/MS method to determine flubendazole and its hydrolyzed and reduced metabolites in eggs and poultry muscle is described. The benzimidazole components were extracted from the two matrices with ethyl acetate after the sample mixtures had been made alkaline. The HPLC separation was performed on an RP C-18 column with gradient elution, using ammonium acetate and acetonitrile as mobile phase. The analytes were detected after atmospheric pressure electrospray ionization on a tandem quadrupole mass spectrometer in MS/MS mode. The components were measured by the MS/MS transition of the molecular ion to the most abundant daughter ion. The overall extraction recovery values for flubendazole, the hydrolyzed metabolite, and the reduced metabolite in eggs (fortification levels of 200, 400, and 800 microg kg(-1)) and muscle (fortification levels of 25, 50, and 100 microg kg(-1)) were, respectively, 77, 78, and 80% and 92, 95, and 90%. The trueness (fortification levels of 400 and 50 microg kg(-1), respectively, for eggs and muscle), expressed as a percentage of the added values for these analytes, was, respectively, 89, 100, and 86 and 110, 110, and 98%. The proposed MS detection method operating in the MS/MS mode is very selective and very sensitive. The limits of detection for flubendazole and its hydrolyzed and reduced metabolites in egg and muscle were, respectively, 0.19, 0.29, and 1.14 microg kg(-1) and 0.14, 0.75, and 0.31 microg kg(-1). The limits of quantification were, respectively, 1, 1, and 2 microg kg(-1) and 1, 1, and 1 microg kg(-1). The discussed method was applied to a pharmacokinetic study with turkeys. Residue concentrations in breast and thigh muscle of turkeys orally treated with flubendazole were quantified. Medicated feed containing 19.9 and 29.6 mg kg(-1) flubendazole was provided to the turkeys for seven consecutive days. For the trial with the recommended dose of 19.9 mg kg(-1), one day after the end of the treatment, the mean sum of the flubendazole plus hydrolyzed metabolite residue values in thigh and breast muscle declined to below the maximum residue limit (50 microg kg(-1)) and were, respectively, 36.6 and 54.1 microg kg(-1). The corresponding values with the higher dose of 29.6 mg kg(-1) were, respectively, 101.7 and 119.7 microg kg(-1). 相似文献
18.
Analyses of chemical residues in animal tissue matrices require multistep sample preparation. To simplify this process, a methodology was developed that combines sorbent extraction and solid-matrix time-resolved luminescence (TRL); it was applied to tetracycline screening in milk. Reported here is an effort to extend its application to tissue matrices, illustrated by oxytetracycline (OTC) screening in catfish muscle. Extraction and enrichment are accomplished by immersing small C18 sorbent strips into tissue homogenates for 20 min, followed by a 3 min rinse in water and a 2 min dip in a reagent solution. After desiccation, TRL is measured directly on the sorbent surface. Tissue particulates no longer interfere via attenuation or scattering, rendering centrifugation and filtration unnecessary. The integrated TRL intensity shows a linear dependence on OTC concentration in the 0-8 microg/g range (R2 = 0.9992) with a 0.026 microg/g limit of detection. To screen OTC at 2 microg/g, the U.S. regulatory tolerance level, a threshold is established at x2-3sigma2, where x2 and sigma2 are the mean and standard deviation, respectively, of the TRL signals from 15 samples fortified at 2 microg/g. Among 45 blind samples randomly fortified at 0-4 microg/g, 41 were screened correctly and 4 negative samples were presumed positive. This method has the potential to improve throughput and save assay costs by eliminating acids, organic solvents, centrifugation, and filtration. 相似文献
19.
Florfenicol (FF) is a broad-spectrum antibiotic used increasingly in aquaculture, livestock, and poultry to treat diseases. To avoid using labor-intensive instrumental methods to detect residues of FF in food and food products, a simple and convenient indirect competitive enzyme-linked immunosorbent assay (ic-ELISA) method for florfenicol's major metabolite, florfenicol amine (FFA), was developed using a polyclonal antibody prepared in this study. FFA was covalently attached to carrier protein as immunogen by using the glutaraldehyde method. The antibodies obtained were characterized by an ELISA method and showed excellent specificity and sensitivity with the 50% inhibition values (IC 50) of 3.34 microg/L for FFA in PBS buffer. In the ELISA, sample extractions were performed by ethyl acetate/ammonium hydroxide (90 + 10, v/v) following combined acid hydrolysis of FF and its known metabolites. The limits of detection (LOD) calculated from the analysis of 20 known negative swine muscle, chicken muscle, and fish samples were 3.08, 3.3, and 3.86 microg/kg (mean + 3 SD), respectively. Recoveries of FFA fortified at the levels of 5, 50, 100, and 300 microg/kg ranged from 64.6 to 124.7%, with coefficients of variation of 11.3-25.8% over the range of FFA concentrations studied. Validation of the ELISA method with FFA-fortified swine muscle at the levels of 10, 50, 100, and 200 microg/kg was carried out using GC, resulting in a similar correlation in swine muscle ( r = 0.97). The results suggest that this ELISA is a specific, accurate, and sensitive method, which is suitable for use as a screening method to detect residues of FFA in animal edible tissues. 相似文献
20.
为同时检测复杂基质中（由猪粪和蘑菇渣混合而成的堆肥原料）3种四环素类抗生素（四环素TC、土霉素OTC和金霉素CTC）及其代谢产物,建立了超高效液相色谱串联质谱检测方法（UPLC—MS／MS）。该方法同时采用pH值=4的Na2EDTA-Mellvaine缓冲溶液和乙腈为提取溶液,经过固相萃取净化后,以乙腈和0．1％的甲酸水溶液为流动相,采用超高效液相色谱柱进行分离,在电喷雾正离子模式下,用四极杆串联质谱仪进行定性和定量分析。3种四环素类抗生素及其代谢产物均在7min内完成分离,总共分析时间为12min。在0-6mg·kg^-1DW（Dryweight）浓度范围内,3种四环素类抗生素及其代谢产物的标准曲线线性良好,线性相关系数R2均大于0．9960,重现l生也较好（n=11,相对标准偏差均小于15％）。在3个加标水平0．2mg·kg^-1DW、1mg·kg^-1DW和4mg·kg^-1DW下,TC、OTC、CTC的回收率分别为71％-89％、66％～94％和66％～84％;去甲基金霉素（DMCTC）的回收率为52％-64％;差向异构产物的回收率在32％～51％之间;脱水产物以及差向脱水产物的回收率均低于30％。3种四环素类抗生素及其代谢产物的检出限和定量限分别在1．668～17．270μg·kg^-1和5．561—45．918μg·kg^-1范围内,表明该方法具有较高的灵敏度。对北京市某露天堆肥场中的样品进行测定发现,TC、OTC、CTC的浓度分别为0．4、1．6、2．9mg·kg^-1,检测到的代谢产物主要为相应的差向异构体,其中差向金霉素（ECTC）的浓度最高,达到2．7mg·kg^-1,和母体的含量水平比较接近,其他代谢产物也有不同程度的检出。 相似文献