共查询到20条相似文献,搜索用时 15 毫秒
1.
R. Halko C. Padron Sanz Z. Sosa Ferrera J. J. Santana Rodríguez 《Chromatographia》2004,60(3-4):151-156
An analytical method was developed to determine the benzimidazole fungicides and their residues (benomyl, carbendazim, thiabendazole and fuberidazole) in real water samples. Analyses were performed by reverse phase (RP) HPLC with direct fluorescence detection with mobile phase methanol:water, 40:60 (v/v) with 0.6% (v/v) ammonia. The extraction of analytes from water samples was performed with the use of micellar systems. Specifically, oligoethylene glycol monoalkyl ether (Genapol X-080) and polyoxyethylene 10 lauryl ether (POLE) were used as extractants. The recoveries of fungicides obtained in spiked water samples ranged from 68% to 94% for Genapol and from 68% to 96% for POLE. The limit of detection (LOD) was lower than 6 g L–1 for carbendazim, 7 g L–1 benomyl, 0.15 g L–1 for thiabendazole and 0.01 g L–1 for fuberidazole in both surfactants. 相似文献
2.
Determination of Abamectin Residues in Avocados by Microwave-Assisted Extraction and HPLC with Fluorescence Detection 总被引:1,自引:0,他引:1
Javier Hernández Borges Lidia M. Ravelo-Pérez Estrella M. Hernández-Suárez Aurelio Carnero Miguel Ángel Rodríguez-Delgado 《Chromatographia》2008,67(1-2):69-75
In this article a new analytical method for the confirmation and quantification of abamectin residues in avocados is described.
The method allows a fast analysis of abamectin homologues using microwave assisted extraction (MAE), solid-phase extraction
(SPE) and high-performance liquid chromatography (HPLC) with fluorescence (FL) detection using trifluoroacetic anhydride (TFAA)
and N-methylimidazole (NMIM) as derivatizing agents. The mobile phase consisted of water, methanol and acetonitrile (5:47.5:47.5
v/v/v) and was pumped at a rate of 1.1 mL min−1 (isocratic elution). Homogenized avocado samples were extracted once with 20 mL acetonitrile:water 4:1 (v/v) in a microwave oven for 26 min at 700 W with a maximum temperature of 80 °C. MAE operational parameters were optimized by
means of an experimental design. Extracts were cleaned using C18 SPE cartridges. Average recoveries of the method at four spiked levels (0.005, 0.01, 0.10 and 1.0 mg kg−1) were found to be in the range 90–100% with good precision (RSD < 12%). The limits of detection (LODs) and quantification
(LOQs) of the whole method were 0.001 and 0.003 mg kg−1, respectively, which are lower than the maximum residue limit (MRL) established by the Spanish and the European legislation
in avocados (0.01 mg kg−1). Several avocado samples previously treated with the pesticide were also analyzed. 相似文献
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4.
M. L. Salazar Cavazos L. Y. Colunga González G. Gallegos de Lerma N. Waksman de Torres 《Chromatographia》2006,63(11-12):605-608
The objective of this work was to develop an analytical HPLC method, using DAD and fluorescence detection, for determination of gatifloxacin in semen. A reversed-phase column was used with 90:10 water-acetonitrile, containing 10 mM TBA and 25 mM citric acid, as mobile phase. Semen was deproteinized with acetonitrile. Recovery was 95 ± 10%. The limits of quantification by DAD and fluorescence were 2.3 and 0.03 μg.mL?1 respectively, with RSD of 3.4% for DAD and 2.8% for fluorescence. The method with fluorescence detection was used for quantification of gatifloxacin in the semen of patients under treatment. 相似文献
5.
Xi Xia Zhiming Xiao Qiushi Huang Lijun Xia Kui Zhu Xiaolin Wang Jianzhong Shen Shuangyang Ding 《Chromatographia》2010,72(11-12):1089-1095
A rapid and sensitive method has been developed for the simultaneous determination of four avermectins and one milbemycin residues in bovine tissue. The isolation of the analytes from muscle and liver samples was accomplished utilizing a pressurized solvent extractor. The optimized extraction procedure using acetonitrile/water (40:60, v/v) as extraction solvent, was automatically carried out at 100 °C and 10 MPa, applying two static cycles for 3 min. The extracts were cleaned up on a C18 solid-phase extraction cartridge and analyzed by liquid chromatography with fluorescence detection after derivatization. Mean recoveries of the five analytes from fortified samples were between 84.8 and 101.8%, with relative standard deviations lower than 10.8%. The limit of detection and quantification were in the ranges of 0.1–0.2 and 0.5–0.6 μg kg–1, respectively. The application of the newly developed method was demonstrated by analyzing bovine meat samples from market. 相似文献
6.
An alternative and practical method is described for simultaneous detection and quantification of the potent hallucinogen lysergic acid diethylamide (LSD) and related compounds in urine and serum samples. The procedure is based on liquid–liquid re-extraction with ethyl acetate and reversed-phase liquid chromatography coupled with fluorescence detection (HPLC–FLD). With detection limits in urine and serum samples of ca 0.07 ng mL–1 for LSD, nor-LSD, and iso-LSD, respectively, the method is well suited to forensic investigations. Application of the method to clinical samples and autopsy material enable selective identification and accurate quantification of LSD and related compounds. Comparison of results with those obtained from an LSD immunoassay (EMIT II) emphasize the need for chromatographic confirmation.Revised: 1 December 2003 and 9 February 2004 相似文献
7.
《液相色谱法及相关技术杂志》2012,35(20):4051-4065
Abstract An automated method for residue analysis of oxolinic acid and flumequine in liver of Atlantic salmon is described. Oxolinic acid and flumequine are extracted from liver with 0.4 M phosphate buffer pH 10 and the extracts are automatically analysed by on-line dialysis and column-switching in an HPLC system. The limit of detection was 4 μg/kg for oxolinic acid and 7 μg/kg for flumequine with fluorescence detection. The on-line combination of dialysis and column-switching HPLC was shown to be a reliable technique for residue control of these drugs in fish liver. 相似文献
8.
A novel, simple, rapid, and accurate method is reported for the determination of 4-hydroxyphenyllactic acid in human urine by high-performance anion-exchange chromatography with fluorescence detection and magnetic solid-phase extraction. The separation and pretreatment conditions for urine were optimized. The isolation of 4-hydroxyphenyllactic acid was performed with isocratic elution with 4?mmol?L?1 sodium hydroxide at 0.45?mL min?1. Fluorescence detection was performed at an excitation wavelength of 277?nm and an emission wavelength of 340?nm. Under the optimized conditions, the linear dynamic range and the limit of detection for 4-hydroxyphenyllactic acid were 0.05–10 and 0.020?mg?L?1, respectively. The recovery for the analyte was from 86.5 to 105.5%, with relative standard derivations less than 4.12%. The method was used for the determination of 4-hydroxyphenyllactic acid in human urine. Statistically significant differences in the 4-hydroxyphenyllactic acid concentration in urine were obtained between healthy control and individuals with breast cancer. 相似文献
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经粉碎的橡胶样品用正己烷及丙酮(1+1)混合溶剂萃取,所得萃取液氮吹至近干后,加正己烷溶解残渣,将溶液经硅胶固相萃取柱净化,吸附于柱上的六溴环十二烷用正己烷-二氯甲烷(1+1)溶液淋洗,洗出液吹氮至近干,用乙腈溶解并用高效液相色谱法测定。选用Zorbax EclipseXDB-C18色谱柱作固定相,用水-乙腈(15+85)溶液作流动相,紫外检测器测定波长为210nm。方法的检出限(3S/N)为1.5mg.kg-1。方法用于橡胶制品中六溴环十二烷的测定,回收率和测定值的相对标准偏差(n=7)分别在83.1%~94.3%和3.6%~6.4%之间。 相似文献
11.
PSA分散固相萃取液相色谱荧光法测定蔬菜和水果中的灭定威 总被引:4,自引:4,他引:4
以PSA分散固相萃取净化,液相色潜柱分离,直接荧光法测定灭定威,研究建立了测定蔬菜、水果中灭定威的分析方法。在仪器最佳测定条件下,灭定威的检出限为2.98pg,在所测定的含量范围内灭定威的含量与峰面积之间的相关系数为1.000,保留时间的卡甘对标准偏差为0.64%:PSA分散固卡相萃取法与氨基柱固相萃取法卡相比,操作简单,基体干扰少,结果准确可靠,重复性好。实际样品中灭定威的平均回收率在89%~112%之间,测得量的相对标准偏差在1.6%~5.6%之间,测定结果令人满意。 相似文献
12.
植物样品中单宁的微波溶出快速测定法研究 总被引:16,自引:0,他引:16
研究了利用微波代替一般的沸水浴处理试样的方法。对不同植物样品中单宁的浸提测定,与常规方法做了对照,并讨论了微波功率、时间、酸度等因素对测定结果的影响。研究表明,此法可大大地缩短测定时间,提高测定效率,节省人力、物力,不污染环境,便于大批量样品的测定,相对标准偏差≤1.4%,测定结果较为满意。为植物样品中单宁的测定,提供了一个快速、简便、准确的分析方法,并可借鉴于其它样品的测定。 相似文献
13.
化妆品样品用甲醇提取使苯甲酸及山梨酸溶于溶剂中,经离心分离,取上层清液,通过反相C18固相萃取小柱纯化。取其流出液经过滤和脱气后,用于高效液相色谱法分析。取20μL进样,在Hypersil C18反相色谱柱(柱温30℃)上进行分离,所用流动相为甲醇与0.02 mol.L-1乙酸铵(15+85)混合溶液,流量为0.8 mL.min-1。采用紫外检测,检测波长为221 nm,测得苯甲酸和山梨酸的检出限(3S/N)分别为0.04,0.08 mg.L-1。用5 mg.L-1的苯甲酸和山梨酸标准溶液作精密度试验,测得两者的相对标准偏差(n=7)分别为2.8%及2.5%,向实际样品中加上述两种酸的标准溶液作回收试验,测得回收率在85.0%~106.7%之间。 相似文献
14.
Wenxiang HU Qingtao PENG Shenjian TAN Jianshe WANG Xunsheng SHAO Peirang Chen Ye CAO 《高等学校化学学报》1998,19(Z1):407
Even though many pharmaceuticals show native chromophoric properties, there are also many important compounds, such as anticholinergic drugs, toxins, steroids and anticancer agents, which are not chromophoric and can not be determined by usual spectra analysis. T-2 toxin is one kind of the compounds. The detection of these compounds by HPLC imposes severe limitation on sensitivity and ofen togather with unacceptable constraints on mobile phase selection. Precolumn or postcolumn derivatization technology by using chromophoric group is often an inexpensive but effective way to overcome this problem, which make these compounds chromophoric and then enhance detcetability of them. For trace analysis, there is a balance to be attained between rigour of sample cleanup and selectivity of detection. Derivatization of target compounds of pharmaceuticals interest offers significant advantages, such as improving selectivity and thus reducing the complexity of the sample cleanup required. 相似文献
15.
A high-performance liquid chromatographic method for the determination of oxolinic acid (OA) residues in muscle tissue and plasma of the cultured fish gilthead seabream (Sparus aurata L.), is described. OA was extracted with ethyl acetate and after centrifugation the combined extracts were evaporated. To the remaining residue 1 mL of the mobile phase was added and the extract was partitioned with n-pentane which then was rejected by aspiration. OA was chromatographed on a Zorbax®SB-C18 column at 50oC and detected by fluorescence detection at λex 327 nm and λem 369 nm. The mobile phase was a mixture of 0.1% trifluoroacetic acid (v/v) pH 2.0 and acetonitrile-methanol 3:2 (v/v) in a combination of 50:50 (v/v) and a flow rate of 1.0 mL min?1, delivered isocratically. Method mean recovery (R%) achieved was 73.7 ± 4.4% (mean ± SD) for blank fortified samples (n=4) range at 50, 100 and 200 μg kg?1 with a RSD=3.3%. The limit of detection (LOD) was 2.0 μg kg?1 oxolinic acid in muscle tissue and plasma and the limit of quantification (LOQ) was 5.0 μg kg?1. The method is fast and suitable to be used with safety and accuracy for the control of OA residues in cultured seabreams and a trained analyst could carry out ready for chromatography more than 50 samples per working day. 相似文献
16.
建立了固相萃取-高效液相色谱法测定化妆品中鞣花酸的含量。样品用甲醇-水(1+1)溶液提取,超声提取10min,以10 000r·min-1转速离心5min,移取5.00mL上清液,经MAX固相萃取柱处理,用甲酸-甲醇(5+95)溶液洗脱。MG C18柱(250mm×4.6mm,5μm)为固定相,以0.2%(体积分数)磷酸-乙腈(18+82)溶液为流动相进行洗脱,检测波长为254nm。线性范围为0.5~100mg·L-1,测定下限(10S/N)为20mg·kg-1,应用该方法对化妆品中鞣花酸的含量进行检测,加标回收率在83.5%~100%之间。 相似文献
17.
Jun Wen Zhenyu Zhu Zhanying Hong Yiwen Wu Yan Fei Mei Lin Guorong Fan Yutian Wu 《Chromatographia》2007,66(1-2):37-41
A cheap, simple and rapid sample preparation method has been developed for quantification of ulifloxacin, the active metabolite
of prulifloxacin in human plasma, by HPLC with fluorescence detection using lemefloxacin as the internal standard. One-step
protein precipitation with 10% perchloric acid (2:1, v/v) on a 200 μL sample was used. The separation was performed at 30 °C on a C18 column using an eluent of acetonitrile-0.5%
triethylamine buffer. The compounds were monitored at λ
ex of 280 nm, λ
em of 425 nm. The calibration curve for ulifloxacin in human plasma was linear over the range 0.01–1.00 μg mL−1. The lower limit of quantification is 0.01 μg mL−1. The intra- and inter-day precision ranged from 3.0 to 6.7%, respectively. The method had been used for clinical pharmacokinetic
studies of prulifloxacin formulation product after oral administration to healthy volunteers.
Jun Wen and Zhenyu Zhu have equal contribution to this work. 相似文献
18.
Haiyang Jiang Shuangyang Ding Fei Xu Sijun Zhao Jihong He Jinfeng Liu Xiaolin Hou Jianzhong Shen 《Chromatographia》2007,66(5-6):411-414
Eprinomectin is a novel and potent antiparasitic animal health drug. An analytical procedure for the determination of EPR
in bovine urine and feces has been developed. The urine sample was centrifuged and alkalized with ammonia following solid
phase extraction. The fecal sample was extracted with acetonitrile, defatted with hexane, cleaned-up using C18 cartridge.
All samples were analyzed by high performance liquid chromatography with fluorescence detection after derivatization with
N-methylimidazole. The limits of detection are 0.5 ng mL−1 and 0.5 ng g−1, respectively. Fortified at 2, 10, 50, and 100 ng mL−1(ng g−1), inter-assay recoveries of EPR in cattle urine and feces were in the range of 87.9–91.5% and 78.6–86.3%, with coefficients
of variation of 5.4–10.2% and 1.4–7.2%, respectively. Intra-assay mean recoveries of the analytes were 82.2–86.5% and 79.6–87.3%,
with coefficients of variation of 7.8–11.5% and 6.3–7.8%, respectively. The method was used to study the excretion of eprinomectin
in bovine urine and feces after subcutaneous administration at a dose of 0.5 mg kg−1. 相似文献
19.
A simple, rapid, and selective high-performance liquid chromatography method for determination of phillyrin in human plasma was developed. After extracting from the plasma samples with ethyl acetate, the analyte was chromatographed on a C18 column with methanol–water (50:50, v/v, pH 2.86) as mobile phase. The fluorescence excitation and emission wavelengths were 277 and 315 nm, respectively. The linear range of the standard curve of phillyrin was 0.0313–8.0 μg mL?1 (r > 0.999). The limit of detection was 6.31 ng mL?1. The average recovery of phillyrin was 101.02% from plasma. The intra- and inter-day variabilities of phillyrin were <10.00%. 相似文献