Determination of furazolidone residues in eggs by HPLC followed by confirmation with a diode-array UV/Vis detector

A sensitive HPLC method for the determination of furazolidone residues in eggs (10-1,000 micrograms/kg) is described. Recovery is about 86%. With the aid of a UV/Vis Diode-Array detector confirmation up to the 15-ppb level was possible. In order to test this method with "real" samples, three laying hens received 30 mg each of furazolidone in feed (single dose). The eggs were collected for five days. After five days traces of furazolidone (5 micrograms/kg) could still be detected.     

SPE-HPLC 紫外双波长测定水果中 10 种农药残留

建立了固相萃取（SPE）-高效液相色谱（HPLC）紫外检测器双波长同时测定草莓、桃和苹果中吡虫啉、啶虫脒、多菌灵、甲基硫菌灵、嘧霉胺、除虫脲、灭幼脲、辛硫磷、苯醚甲环唑和阿维菌素10种农药残留的分析方法。水果样品用乙腈作为提取溶剂经高速匀浆提取,提取液经LC-NH2固相小柱净化富集,以甲醇、水和乙腈作为梯度洗脱的流动相,采用Shiseido CAPCELL PAK MG ⅡC18色谱柱（250 mm×4.6 mm,5 μm）分离,选择270 nm和245 nm双波长进行目标化合物的检测。结果表明：10种农药在0.05-1.0 mg/kg范围内具有良好的线性关系（0.9834-0.9992）,检出限为0.005-0.030 mg/kg,定量限为0.020-0.098 mg/kg。0.05、0.10、0.20 mg/kg添加水平的回收率为69.82-88.95%,86.77-110.61%和89.74-110.62%;相对标准偏差（RSD）为6.52-13.24%,5.21-10.32%和3.56-9.88%。与其他方法相比,具有简便、准确、节约试剂和能耗低等优点,适合水果中10种农药残留的同时测定及定量分析。     

同时检测畜禽肉中呋喃唑酮、地塞米松残留高效液相色谱法的建立

为建立畜禽肉中呋喃唑酮、地塞米松HPLC检测方法。经试验,得到的色谱条件为流动相:乙腈-水(40+60);检测波长:240nm;流速:1.0mL/min。采用该方法检测了市售畜禽肉中呋喃唑酮、地塞米松的残留量,结果表明:该方法分离效果良好,平均回收率范围85.41%～95.2%,相对标准偏差为2.0%～4.5%,最低检出限达1.0～2.0μg/mL,说明该方法灵敏、准确、精密、无杂质干扰,可以用于肉品中呋喃唑酮、地塞米松残留的检测。     

高效液相色谱法测定甘蓝中多茵灵残留

建立一种测定甘蓝中多茵灵残留量的高效液相色谱分析法.甘蓝样品经乙腈提取,弗洛里硅土固相萃取柱净化后,经C18色谱柱分离,以V(甲醇):V(水)=7:3为流动相,在0.3 mL/min务件下洗脱,于286 nm波长下用紫外检测器进行检测.结果表明,多菌灵峰面积与其浓度呈良好线性关系,最低栓出限可达0.008 mg/L,回收率为84.8%～89.4%,相对标准偏差低于2.7%.     

荧光胺柱前衍生高效液相色谱法测定牛肉中的盐酸克伦特罗

建立了高效液相色谱-荧光检测器测定牛肉中的盐酸克伦特罗的方法。样品通过提取、净化、荧光胺柱前衍生化,用配有荧光检测器的高效液相色谱仪测定,外标法定量。方法检出限为0.5μg/g,在2.0～100ng/mL范围内,线性相关系数R为0.9996。在2.0、10、20μg/g3种浓度添加水平,盐酸克伦特罗的回收率为85.15%～93.25%,相对标准偏差为2.81%～3.16%。该方法重现性好、灵敏度高、特异性强,可用于牛肉中盐酸克伦特罗残留的检测。     

电子捕获检测器测定粮食中三唑酮残留量

建立了气相色谱法一电子捕获检测器测定粮食中三唑酮农药残留量的方法,并对方法的最低检测限、校准曲线、加标回收率、精密度、准确度等指标进行了确认。结果表明,采用该方法所测定的三唑酮农药残留量在DB-1701毛细管柱上得到了很好的分离,且方法准确、快速、灵敏,完全符合实际应用需要。     

Determination of acrylamide in processed foods by column-switching HPLC with UV detection

A simple and convenient analytical method for the determination of acrylamide in processed foods was established. Acrylamide was extracted with water in an ultrasonic bath. The extract was passed through an OASIS HLB cartridge and the eluate was injected into the HPLC system using a column-switching technique. The HPLC system consisted of two pumps, two 6-port-2-position valves, two columns and a UV detector. At first, the sample solution was chromatographed on an ODS column with a mobile phase of water, then the flow of the mobile phase was switched using a 6-port-2-position valve, and the acrylamide peak fraction was introduced into an aqueous gel permeation column (analytical column). The fraction was chromatographed again on the analytical column with a mobile phase of water, and the eluate was monitored with a UV detector (205 nm). The recoveries of acrylamide from potato chips, fried potato, croquette and instant noodle fortified at levels of 50 to 1,000 micrograms/kg were 93.1 to 101.5% and the coefficient of variation was 1.5 to 5.2%. The detection limit corresponded to 10 micrograms/kg in processed foods. Forty-six samples, potato chips (11), fried potato (10), croquette (20) and instant noodle (5), were analyzed by this method. The acrylamide level was 67-4,499 micrograms/kg for potato chips, 125-1,183 micrograms/kg for fried potato, nd-255 micrograms/kg for croquette and nd-151 micrograms/kg for instant noodle.     

Determination of Safrole and Isosafrole in Ham by HPLC with UV Detection

An improved method has been developed for the determination of safrole and isosafrole in meat. To ham were added known amounts (5–100 ppm) of either compound or mixtures of both. The samples were extracted with hexane/ethyl acetate (95/5, v/v) by a dry column procedure, and the eluate was analyzed by HPLC with UV detection. Recoveries ranged from 91–102% for the individual components and from 93–100% for mixtures. The improved method requires less analysis time and instrumentation and is more sensitive than a previous method.     

养殖水产品中四环素类抗生素残留的高效液相色谱测定法

建立了HPLC检测养殖水产品中四环素类抗生素残留的方法,采用乙酸乙酯(Imol/L) 乙酸镁(0.05mol/L) EDTA(0.001mol/L)的混合液提取样品中的四环素、土霉素、全霉素.以上述混合液-甲醇(72:28,v/v)为流动相,流速1mL/min,检测波长370hm.在0.05～1.0mg/L范围内峰面积与抗生素浓度呈良好的线性关系(r＞0.99).检出限分别为0.013mg/g(土霉素)、0.016mg/g(四环素)、0.014mg/g(金霉素),平均加标回收率分别91.2%(土霉素)、88.5%(四环素)、95.6%(金霉素),精密度(RSD)小于5%.     

Determination of phenolic compounds in alcoholic beverages by HPLC with an electrochemical detector

A method has been developed for the quantitative determination of phenolic lignin degradation products in alcoholic distillates. After diluting the samples with the eluent (1:5-1:10, v/v) the phenolic compounds are separated by high-pressure liquid chromatography and detected by an electrochemical detector at +1.3 V. To identify the compounds the k'-values and the hydrodynamic voltammograms of the samples are compared with those of the standard solution. Several distilled alcoholic beverages were analysed. The content of phenolic compounds was found to vary between 0.15 and 7.7 mg/l. The detection limits were 0.3-0.9 ng.     

Determination of glycarbylamide residues in chicken tissues by HPLC with post-column reaction

A newly developed HPLC method for determination of glycarbylamide (GB) in chicken liver was applied to other tissues (muscle, fat and kidney). The recoveries of GB in muscle, fat and kidney were 87.2% (CV 0.5), 91.3% (CV 4.7), 79.7% (CV 1.0), respectively. The detection limit of GB was 0.01 ppm. GB concentrations were determined by this method in tissues (muscle, fat, liver and kidney) from chickens sacrificed 5 days after oral administration of GB mixed in feed at 60 mg/kg of feed for 7 days. GB was not detected in these chicken tissues.     

Determination and depletion of amoxicillin residues in eggs

Eggs were used to study the determination and depletion of amoxicillin (AMO) residues after oral dosing hens (25.0 mg kg^–1, 50.0 mg kg^–1 body weight), once daily for five days. A reverse-phase high-performance liquid chromatography with fluorescence detection (RP-HPLC-FLD) method was developed to determine AMO residues in albumen, yolk and whole egg. By using pre-column derivatisation, an improved liquid–liquid extraction procedure was developed for sample preparation. AMO were extracted from eggs with acetonitrile. The extract solution was extracted using saturated methylene chloride. The supernatant was reacted with salicylaldehyde under acidic and heating conditions. Limits of detection (LODs) were 1.2 ng g^–1 and limits of quantification (LOQs) were 3.9 ng g^–1 for AMO. Recoveries of AMO from samples fortified at levels of 5.0–125.0 ng g^–1 ranged from 79.1% to 88.5% in albumen, 78.6–83.6% in yolk and 78.3–85.1% in whole egg, with coefficients of variation of ≤7.3%. The maximum concentrations of AMO in albumen, yolk and whole egg were found to occur at 1.5, 2.5, 1.5 days after withdrawal of medication respectively. AMO was not detectable in albumen at 7.5 days after final administration of AMO, at 10.5–11.5 days in yolk and 10.5 days in whole egg after administration of two oral doses. The method was applied during the residue study of AMO in order to formulate a reasonable withdrawal period to ensure food safety.     

高效液相色谱法测定水产品中呋喃西林的研究

建立了高效液相色谱测定水产品中呋喃西林残留量的方法。通过对比不同有机溶剂的提取效果,表明使用单溶剂提取回收率均不高,采用丙酮和二氯甲烷的混合溶液提取效果更好,其中比例为3∶7时最佳。比较了振荡法、超声波法和超声波加热法等的提取能力,结果表明,超声波加热法提取效果最好。以丙酮-二氯甲烷作为提取剂、超声波加热（35kHz,强度100%,40℃）进行提取,提取时间15min、提取2次,提取率可达90%以上,方法回收率在75%～100%之间,相对标准偏差小于10%,检测限能达到0.5μg/kg。本方法操作简便,回收率较高,稳定性好。     

高效液相色谱-蒸发光散射检测器测定脂肪酸和甘油酯的含量

建立了一种利用反相高效液相色谱-蒸发光散射检测、通过梯度洗脱测定油脂中脂肪酸、单甘酯、二甘酯与三甘酯含量的方法,色谱柱是C18反相柱,流动相为乙腈(0.05%醋酸V/V)-二氯甲烷,流速1.0 mL/min;蒸发光散射检测器漂移管温度70℃,载气流速1.7L/min.各物质色谱峰面积的自然对数与浓度的自然对数呈良好的线性关系,精密度RSD为0.43%～2.75%,最低检测限为0.02～0.04μg,回收率测定值为93.2%～104.5%.该方法不仅可以准确、快速地定量、定性分析各类混合脂肪酸甘油酯和游离脂肪酸,而且还可以分离具有立体异构的单甘酯和二甘酯.     

Determination of piperazine in hen eggs with HPLC following oral administration

After oral administration of piperazine citrate to hens, this antihelmintic agent appeared unchanged in the eggs. After a therapeutic dose of ca. 0.9 g piperazine citrate per hen, a maximum level of 1.5 mg piperazine/kg egg was found two days after the application. The elimination half-life was 29 h and piperazine was found in the eggs up to 17 days after administration (limit of detection: 1 microgram/kg). Piperazine determination was performed by HPLC of the dansylderivative after clean-up by TLC.     

Determination of aflatoxins in eggs,milk, meat and meat products using HPLC fluorescent and UV detectors

Raw and pasteurised sheep’s, cow’s and goat’s milk, eggs, and beef samples from different local markets in Jordan were collected during a period of 5 months (January through May 2007) and examined for aflatoxins B1(AFB1), B2(AFB2), G1(AFG1), G2(AFG2), M1(AFM1) and M2(AFM2). The samples were analysed with high performance liquid chromatography (HPLC) using UV and Fluorescent detectors. The analysed samples of milk collected in January were found to contain 0.56 μg L⁻¹ AFM1 and 0.1 μg L⁻¹ AFM2 whilst, the concentration of AFM1 and AFM2 was < 0.05 μg L⁻¹ for milk samples collected between March and May. The AFB1, AFB2, AFG1 and AFG2 contents in the analysed food products ranged from 1.10 to 8.32 μg L⁻¹ and 0.15 to 6.36 μg L⁻¹ in imported and fresh meat samples collected during March, respectively. The mean recovery for the HPLC method was 92% to 109% and the quantification levels were 50 ng L⁻¹ for AFM1 and AFM2. The AFM1 was found in 10% of the tested samples with concentrations between 0.08 and 1.1 μg kg⁻¹ and AFM2 was only found in 1.82% of the tested samples with a level of 0.1 μg kg⁻¹. The AFM1 levels in the examined foods were higher than the maximum level of AFM1 in liquid milk set by the European Community and Codex Alimentarius of 50 ng L⁻¹.     

高效液相色谱法检测蔬菜中百菌清及其代谢产物的方法研究

建立了同时检测蔬菜中百菌清(CHT)及其代谢产物(4-羟基百菌清,CHT-OH)残留的高效液相色谱分析法。样品经丙酮提取,弗洛里硅土柱净化浓缩后以适量甲醇定容,HPLC紫外检测器检测,以C18色谱柱分离,甲醇∶水(90∶10,V/V)为流动相,流速为0.7mL/min,检测波长240nm。结果表明,百菌清、4-羟基百菌清的检测线性范围分别为0.05～10mg/kg和0.01～10mg/kg,相关系数r=0.9999。方法检出限分别为0.012mg/kg和0.005mg/kg,二者的平均加标回收率为83.5%～121.3%,RSD为2.4%～4.6%,该方法可用于市售蔬菜样品的测定。     

液相色谱双检测器串联法测定农产品中农药残留

建立了采用高效液相色谱-紫外-荧光检测器串联法测定农产品中12种农药残留的方法。采用乙腈提取,使用氨基固相萃取小柱净化,通过液相色谱柱及变换波长等各种色谱条件优化,紫外检测器检测吡虫啉、多菌灵、除虫脲、灭幼脲、辛硫磷,荧光检测器测定经柱后衍生的氨基甲酸酯类农药残留。12种农药在0.05～4mg/kg范围内线性良好,平均回收率在73.0%～108%之间,RSD为0.2%～7.1%,检出限为0.001～0.03mg/kg。方法快速、经济,为农产品中农药残留检测增加一种新思路。     

超声辅助分散液液微萃取-高效液相色谱法测定蜂蜜中溴氰菊酯残留

采用超声辅助分散液液微萃取技术结合高效液相色谱法测定蜂蜜中的溴氰菊酯。蜂蜜样品用乙腈∶水(1∶4,v/v)混合溶液提取,加入氯仿萃取,超声,离心,得到沉积相,进行HLPC分析。溴氰菊酯在10~1000μg/kg范围内线性良好,相关系数r=0.9998,富集倍数高达600倍。当蜂蜜样品的加标浓度为10、50、100μg/kg时,加标回收率为82.6%~97.3%,相对标准偏差为2.1%~3.8%。蜂蜜样品中溴氰菊酯的检出限为8μg/kg,定量限为40μg/kg。本方法具有简便快捷、准确灵敏、萃取效率高、有机溶剂消耗少等特点,可成功地应用于蜂蜜中溴氰菊酯残留的测定。     

Determination of vitamin K1 content in olive oil,chard and human plasma by RP-HPLC method with UV–Vis detection

The contents of phylloquinone (Vitamin K₁) were investigated in olive oil, chard and human plasma based on a reversed phase high performance liquid chromatographic method with acetonitrile/dichloromethane/methanol (60:20:20, v/v/v) as eluent in a C₁₈ μ-Bondapak column (10 μm, 300 × 3.9 mm) at 20 °C. Detection was by UV–Vis detector at 248 nm. In olive oil, the mean content of phylloquinone ranged from 12.7 to 18.9 μg/100 g, in chard ranged from 65.5 to 77.5 μg/100 g. In human plasma, phylloquinone content varied between 0.22 and 0.56 ng/ml.