Journal - Association of Official Analytical Chemists最新文献

英文中文

Bacillus stearothermophilus disk assay for determining ampicillin residues in fish muscle. 鱼肌肉中氨苄西林残留量测定的嗜热脂肪芽孢杆菌圆盘试验。

Journal - Association of Official Analytical Chemists

Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.910

S. M. Plakas, A. DePaola, M. Moxey

The Bacillus stearothermophilus disk assay for penicillin in milk (AOAC official method) was adapted for the determination of ampicillin in fish muscle. The method was evaluated in 2 species of cultured fish: channel catfish and striped bass. Recoveries of ampicillin ranged from 99 to 104% when muscle specimens from both species were spiked at concentrations of 0.025-1.00 micrograms/g. The lower limit of determination (LOD) was 0.025 micrograms/g. The assay was applied to monitor the elimination of ampicillin from the muscle of striped bass after intravascular administration (dosage of 10 mg/kg body weight). The mean concentrations in the muscle declined from 1.160 micrograms/g at 2 h to 0.063 micrograms/g at 18 h. The half-life of ampicillin in the muscle was 3.6 h. Ampicillin concentrations were below LOD at 24 h. No inhibitory activity was observed in the muscle of control fish.

采用乳中青霉素嗜热脂肪芽孢杆菌圆盘法(AOAC官方方法)测定鱼肌中氨苄西林。该方法在2种养殖鱼类中进行了评价:槽鲶和条纹鲈鱼。当两个物种的肌肉标本在0.025-1.00微克/克的浓度下加标时，氨苄西林的回收率为99 - 104%。检测下限(LOD)为0.025微克/克。本实验用于监测血管内给药(剂量为10 mg/kg体重)后氨苄西林在条纹鲈鱼肌肉中的消除情况。肌肉中氨苄西林的平均浓度从2 h时的1.160微克/g下降到18 h时的0.063微克/g。氨苄西林在肌肉中的半衰期为3.6 h, 24 h时氨苄西林浓度低于LOD。对照鱼肌肉中未观察到氨苄西林的抑制活性。

引用次数: 5

An analytical survey of aflatoxins in tissues from swine grown in regions reporting 1988 aflatoxin-contaminated corn. 1988年玉米受黄曲霉毒素污染地区猪组织中黄曲霉毒素的分析调查。

Journal - Association of Official Analytical Chemists

Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.897

R. Stubblefield, J. P. Honstead, O. Shotwell

A joint project was undertaken by the Food Safety and Inspection Service (FSIS) and the Agriculture Research Service branches of the U.S. Department of Agriculture to determine the presence of aflatoxins in the U.S. meat supply during a drought year. In 1988, high incidences of aflatoxins occurred in corn grown in regions of the Midwest, Southeast, and South. Six states were identified as having serious aflatoxin contamination in their corn crop: Virginia, North and South Carolina, Texas, Iowa, and Illinois. Swine liver and pillars of diaphragm (muscle) tissues were sampled by federal FSIS Inspectors in plants located in these states. A worstcase sampling plan was conducted. Samples were taken in January 1989 from hogs fed corn soon after harvest and in April 1989 from hogs fed corn originally stored and then fed in the spring. A modification of the official AOAC method for the thin-layer chromatography (TLC) determination of aflatoxins in animal tissue was used to permit quantitation by LC with fluorescence detection. The official AOAC TLC confirmation of identity method was used to confirm all positive samples with B1 concentrations greater than 0.04 ppb and M1 concentrations greater than 0.1 ppb. Sixty samples in the January group and 100 samples in the April group were assayed. Concentrations of aflatoxins B1 and M1 in the first group of pig livers ranged from 0.04 to 0.06 ppb. The identity of aflatoxin B1 was confirmed in all positive samples. Aflatoxin M1 could not be confirmed in any of the positive liver samples because the method was insufficiently sensitive for this aflatoxin.(ABSTRACT TRUNCATED AT 250 WORDS)

美国农业部下属的食品安全检验局(FSIS)和农业研究服务局开展了一项联合项目，以确定干旱年份美国肉类供应中是否存在黄曲霉毒素。1988年，美国中西部、东南部和南部地区种植的玉米中黄曲霉毒素的发病率很高。六个州的玉米作物被确认存在严重的黄曲霉毒素污染:弗吉尼亚州、北卡罗来纳州和南卡罗来纳州、德克萨斯州、爱荷华州和伊利诺伊州。猪肝和横膈膜(肌肉)组织柱由联邦FSIS检查员在这些州的工厂取样。进行了最坏情况抽样计划。1989年1月从收获后不久饲喂玉米的猪身上采集样本，1989年4月从最初储存、然后在春季饲喂玉米的猪身上采集样本。对动物组织中黄曲霉毒素薄层色谱(TLC)测定的官方AOAC方法进行了改进，采用荧光检测的LC定量方法。所有B1浓度大于0.04 ppb、M1浓度大于0.1 ppb的阳性样品均采用官方AOAC薄层鉴别法进行鉴定。1月组60份，4月组100份。第一组猪肝中黄曲霉毒素B1和M1的浓度范围为0.04 ~ 0.06 ppb。所有阳性样本均确认为黄曲霉毒素B1。由于该方法对黄曲霉毒素不够敏感，因此无法在任何阳性肝脏样本中确认黄曲霉毒素M1。(摘要删节250字)

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引用次数: 14

Separation and determination of diesel contaminants in various fish products by capillary gas chromatography. 毛细管气相色谱法分离测定各种鱼类产品中柴油污染物。

Journal - Association of Official Analytical Chemists

Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.986

J. M. Newton, B. Rothman, F. Walker

A semiquantitative capillary column gas chromatographic method is described for the determination of diesel fuel contamination in various canned seafood products. The diesel contaminants are separated from the fish sample by steam distillation, with little carry-over of interfering intrinsic materials such as fish oils. The diesel fuel is extracted from the condensate with n-hexane, and the extract is analyzed on an SPB-1 fused silica capillary column. The efficiency of recovery of diesel fuel added to canned seafood at levels of 40-400 ppt ranged from 72 to 102%. With the additional step of concentrating the hexane extract, the sensitivity of this procedure may be increased at least 10-fold. This procedure can detect the differences among diesel fuel grades No. 1, 2, and 5, and variations within diesel grade No. 2, and thus may be useful in determining the type of petroleum contaminants present in various canned fish products.

介绍了一种半定量毛细管柱气相色谱法测定各种海鲜罐头产品中柴油污染的方法。柴油污染物通过蒸汽蒸馏从鱼样品中分离出来，几乎没有携带干扰的固有物质，如鱼油。用正己烷从凝析液中提取柴油，并在SPB-1型熔融石英毛细管柱上进行分析。海产品罐头中添加40 ~ 400 ppt水平的柴油，其回收率为72 ~ 102%。随着浓缩己烷萃取物的额外步骤，该程序的灵敏度可能增加至少10倍。该程序可以检测1、2、5号柴油燃料等级之间的差异，以及2号柴油等级内部的变化，因此可以用于确定各种罐头鱼产品中存在的石油污染物的类型。

引用次数: 4

Residue analysis of glyphosate and its principal metabolite in certain cereals, oilseeds, and pulses by liquid chromatography and postcolumn fluorescence detection. 利用液相色谱法和柱后荧光检测法对某些谷物、油籽和豆类中的草甘膦及其主要代谢物进行残留分析。

Journal - Association of Official Analytical Chemists

Pub Date : 1991-09-01

Y Y Wigfield, M Lanouette

A postcolumn liquid chromatographic method to determine the extractable residues of glyphosate (GLYPH) and its principal metabolite, (aminomethyl)phosphonic acid (AMPA), in various cereals and beans is described. The finely ground sample is extracted with a mixture of chloroform and water, and the resulting aqueous layer is passed through a cation exchange column. The eluate is adjusted to pH 7-10 and passed through an anion exchange column. The second column is eluted with 0.3M HCl solution and the resulting acidic eluate is analyzed with liquid chromatography coupled with postcolumn fluorescence detection. The mean recoveries for GLYPH in barley, canola, dry pea, flax, soybean, wheat, and white bean ranged from 90.0 to 98.1%, with coefficients of variation (CV) from 2.9 to 10.0% and limits of detection (LOD) from 0.07 to 0.14 ppm. Similarly, mean recoveries for AMPA in the same crops ranged from 87.4 to 98.9%, with CV from 4.6 to 7.7 and LOD from 0.05 to 0.12 ppm. Using this method, an analyst can routinely analyze 6 samples per 1.5 days. The advantages of this procedure are discussed.

介绍了一种柱后液相色谱法，用于测定各种谷物和豆类中草甘膦（GLYPH）及其主要代谢物（氨甲基）膦酸（AMPA）的可萃取残留量。用氯仿和水的混合物萃取磨碎的样品，所得水层通过阳离子交换柱。洗脱液的 pH 值调至 7-10 并通过阴离子交换柱。第二个色谱柱用 0.3M HCl 溶液洗脱，得到的酸性洗脱液通过液相色谱法和柱后荧光检测进行分析。大麦、油菜、干豌豆、亚麻、大豆、小麦和白豆中 GLYPH 的平均回收率为 90.0% 至 98.1%，变异系数 (CV) 为 2.9% 至 10.0%，检测限 (LOD) 为 0.07% 至 0.14 ppm。同样，相同作物中 AMPA 的平均回收率为 87.4% 至 98.9%，CV 为 4.6% 至 7.7%，LOD 为 0.05% 至 0.12 ppm。使用这种方法，分析师可以在 1.5 天内对 6 个样品进行常规分析。本文讨论了这一方法的优点。

引用次数: 0

Quantitation of the nitrosamine 2-ethylhexyl-4-(N-methyl-N-nitrosoamino) benzoate (NPABAO) in sunscreen products. 防晒产品中亚硝胺2-乙基己基-4-(n -甲基-n -亚硝基氨基)苯甲酸酯(NPABAO)的含量测定。

Journal - Association of Official Analytical Chemists

Pub Date : 1991-09-01 DOI: 10.1093/JAOAC/74.5.766

T. Meyer, J. B. Powell

We have devised a method to quantitate the nitrosamine, 2-ethylhexyl-4-(N-methyl-N-nitrosoamino) benzoate (NPABAO), in commercial products containing the sunscreen ingredient, Padimate O. The method involves a minimum of cleanup steps to afford a nonaqueous extract from product emulsions suitable for analysis by a liquid chromatograph interfaced to a thermal energy analyzer (LC/TEA). The method is applicable to lotions, creams, and gels. Oils are normally soluble in the mobile phase and can be analyzed directly on the LC/TEA without additional cleanup procedures. The method has a minimum detectable limit of about 30 ppb and yields greater than 80% recovery. It is highly reproducible and generates no NPABAO artifactually prior to quantitation on the LC/TEA. Application of the method to 22 different commercial product formulas disclosed that the level of NPABAO in each of the products is below 250 ppb, with 18 of the products containing less than 100 ppb. Of interest was the observation that musk ketone, a common fragrance constituent, produces a false-positive TEA response that can interfere with accurate analysis of NPABAO content in typical commercial products.

我们设计了一种方法来定量含有防晒成分帕二酸o的商业产品中的亚硝胺，2-乙基己基-4-(n -甲基-n -亚硝基氨基)苯甲酯(NPABAO)。该方法涉及最少的清理步骤，从产品乳状液中获得适合通过液相色谱仪与热能分析仪(LC/TEA)接口进行分析的非水提取物。该方法适用于乳液、面霜和凝胶。油通常可溶于流动相，可以直接在LC/TEA上进行分析，而无需额外的清理程序。该方法的最小检测限约为30 ppb，回收率大于80%。该方法重现性好，在LC/TEA定量前不会人为产生NPABAO。将该方法应用于22种不同的商业产品配方，发现每种产品中的NPABAO含量低于250 ppb，其中18种产品的含量低于100 ppb。令人感兴趣的是观察到麝香酮，一种常见的香料成分，会产生假阳性的TEA反应，从而干扰对典型商业产品中NPABAO含量的准确分析。

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引用次数: 2

Determination of Mirex in human blood serum containing polychlorinated biphenyls by using packed column gas chromatography. 填充柱气相色谱法测定含多氯联苯的人血清中灭雷克斯的含量。

Journal - Association of Official Analytical Chemists

Pub Date : 1991-09-01 DOI: 10.1093/JAOAC/74.5.875

M. P. Korver, V. Burse, L. Needham, V. Green, D. L. Gray, M. Rouse, T. Shelly., B. Mortensen

An analytical method has been developed that uses electron capture/gas-liquid chromatography to determine Mirex in serum containing polychlorinated biphenyls (PCBs) (Aroclor 1260). With this method, 0.2 ppb Mirex can be determined in 4 mL serum that also contains 10 ppb PCBs. The method provides approximately 70% recovery of Mirex at 1.0 and 3.5 ppb. The coefficients of variation are 4.5 and 4.6% at 1.0 and 3.5 ppb, respectively. In a cooperative study with the Ohio Department of Health, the Centers for Disease Control used this method to determine the extent of exposure of Salem, OH, residents to Mirex. Confirmation of Mirex was obtained by using high resolution gas chromatography and high resolution mass spectrometry.

开发了一种电子捕获/气液色谱法测定含多氯联苯(PCBs) (Aroclor 1260)血清中咪雷克斯的分析方法。使用该方法，在含有10 ppb多氯联苯的4 mL血清中可以测定0.2 ppb的Mirex。该方法在1.0和3.5 ppb下可提供约70%的Mirex回收率。在1.0和3.5 ppb下，变异系数分别为4.5和4.6%。在与俄亥俄州卫生部的一项合作研究中，疾病控制中心使用这种方法来确定俄亥俄州塞勒姆居民对米雷克斯的暴露程度。采用高分辨率气相色谱法和高分辨率质谱法对Mirex进行确证。

引用次数: 2

Liquid chromatographic determination of chlortetracycline hydrochloride in ruminant and poultry/swine feeds. 反刍动物和家禽/猪饲料中盐酸氯四环素的液相色谱测定。

Journal - Association of Official Analytical Chemists

Pub Date : 1991-09-01 DOI: 10.1093/JAOAC/74.5.780

D. C. Holland, K. C. Faul, J. Roybal, R. K. Munns, W. Shimoda

A liquid chromatographic (LC) method is described for the determination of chlortetracycline hydrochloride (CTC) in poultry/swine and ruminant feeds in the 10-100 ppm range and in premix. CTC is extracted from ground feed/premix with acidified acetone, and the extract is filtered through a Millex-HV filter or disposable C18 column. The filtrate is partitioned with methylene chloride when additional cleanup is necessary. A Nova-Pak C18 column is used for LC separation with determination at 370 nm. The average recovery of CTC from premix was 95% with a standard deviation (SD) of 1.70 and a coefficient of variation (CV) of 1.79%. The overall average recovery from feeds was 77% with an SD of 3.18 and a CV of 4.10%.

建立了禽/猪和反刍动物饲料中盐酸氯四环素(CTC)的液相色谱测定方法，测定范围为10-100 ppm。CTC从研磨料/酸化丙酮预混料中提取，提取液通过Millex-HV过滤器或一次性C18柱过滤。当需要额外的清理时，滤液用二氯甲烷分隔。采用Nova-Pak C18色谱柱进行色谱分离，测定波长为370 nm。CTC的平均回收率为95%，标准差(SD)为1.70，变异系数(CV)为1.79%。饲料的总体平均回收率为77%，SD为3.18,CV为4.10%。

引用次数: 8

Gas chromatographic determination of captan, folpet, and captafol residues in tomatoes, cucumbers, and apples using a wide-bore capillary column: interlaboratory study. 用宽孔毛细管柱气相色谱法测定番茄、黄瓜和苹果中上尉、上尉和上尉醇残留量:实验室间研究。

Journal - Association of Official Analytical Chemists

Pub Date : 1991-09-01

D M Gilvydis, S M Walters

An interlaboratory study of the determination of captan, folpet, and captafol in tomatoes, cucumbers, and apples was conducted by 4 laboratories using wide-bore capillary column gas chromatography with electron capture detection. The 3 fungicides were determined using the Luke et al. multiresidue method modified to include additional solvent elution in the optional Florisil column cleanup step used with this method. The crops were fortified with each fungicide at 3 levels per crop. Mean recoveries ranged from 86.2% for a 25.1 ppm level of captan in apples to 115.4% for a 0.288 ppm level of captafol in apples. Interlaboratory coefficients of variation ranged from 3.4% (24.7 ppm folpet) to 9.7% (0.243 ppm captafol) for tomatoes; from 2.8% (2.0 ppm captafol) to 8.2% (24.8 ppm captan) for cucumbers; and from 1.5% (0.234 ppm folpet) to 22.1% (0.266 ppm captafol) for apples.

采用大口径毛细管柱气相色谱-电子捕获检测法，对番茄、黄瓜和苹果中的队长、队长、队长酚进行了实验室间的测定研究。采用Luke等人的多残留法测定这3种杀菌剂，该方法在可选的Florisil柱清洗步骤中加入了额外的溶剂洗脱。每种杀菌剂每株作物强化3级。平均回收率从25.1 ppm苹果中队长醇的86.2%到0.288 ppm苹果中队长醇的115.4%不等。番茄的实验室间变异系数为3.4% (24.7 ppm皂角醇)至9.7% (0.243 ppm皂角醇);黄瓜的含硫量由2.8%(百万分之2.0)增至8.2%(百万分之24.8);苹果从1.5% (0.234 PPM乙醇)到22.1% (0.266 PPM乙醇)。

引用次数: 0

Validation of methods used in the Florida Department of Agricultural and Consumer Services' Chemical Residue Laboratory. 佛罗里达州农业和消费者服务部化学残留实验室使用的方法的验证。

Journal - Association of Official Analytical Chemists

Pub Date : 1991-09-01 DOI: 10.1093/JAOAC/74.5.868

G. A. Parker

Very few methods for detecting residues of pesticides in food or agricultural samples have undergone rigorous colloborative study and possess official AOAC status. The Chemical Residue Laboratory has formalized a method validation scheme to use when incorporating or developing new, unofficial methods. These methods are validated by assessing certain performance parameters: scope, specificity, linear range, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ). For accuracy and precision assessment, 12 replicate fortifications must yield recoveries within the range of 70-120% with a coefficient of variation (CV) that compares favorably to the Horwitz CV. LOD and LOQ are equivalent to 3 and 10 times, respectively, the background signal contributed by a sample matrix blank. This criterion that we use for LOD/LOQ is not universal. In fact, because of differing definitions, we have encountered difficulties in enforcing a tolerance by using a registrant's method. This paper also presents an example of our method validation scheme, using a recent method development project for detecting sulfamethazine in raw milk. The sulfamethazine project also revealed unanticipated personnel problems, underscoring the importance of the human factor in quality assurance.

很少有检测食品或农业样品中农药残留的方法经过严格的合作研究并获得官方的AOAC地位。化学残留实验室已正式制定了一套方法验证方案，以便在合并或开发新的非官方方法时使用。这些方法通过评估某些性能参数来验证:范围、特异性、线性范围、准确度、精密度、检出限(LOD)和定量限(LOQ)。对于准确度和精密度评估，12个重复强化的回收率必须在70-120%的范围内，变异系数(CV)优于霍维茨CV。LOD和LOQ分别相当于一个样本矩阵空白所贡献的背景信号的3倍和10倍。我们用于LOD/LOQ的这个标准并不是通用的。事实上，由于不同的定义，我们在使用注册者的方法来实施容忍度时遇到了困难。本文还介绍了我们的方法验证方案的一个例子，使用最近的方法开发项目检测原料奶中的磺胺乙胺。磺胺乙嘧啶项目还暴露了意想不到的人员问题，强调了人的因素在质量保证中的重要性。

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引用次数: 17

Competitive direct enzyme-linked immunosorbent screening assay for the detection of sulfamethazine contamination of animal feeds. 竞争性直接酶联免疫吸附筛选法检测动物饲料中磺胺乙胺污染。

Journal - Association of Official Analytical Chemists

Pub Date : 1991-09-01

D E Dixon-Holland, S E Katz

A sensitive screening method has been developed for detecting sulfamethazine (SMZ) contamination of feeds by using either polyclonal or monoclonal antibodies and a direct competitive enzyme-linked immunosorbent screening assay (ELISA). Feed samples of 25.0 g are extracted with 0.5N HCl and centrifuged. The extract is adjusted to pH 7.0 with 3.0N NaOH and recentrifuged. This pH-adjusted extract is used in the ELISA. Levels as low as 0.004 micrograms SMZ/g feed were detected in supplemented extracts by polyclonal antibodies; levels of 0.4 micrograms SMZ/g feed were detected by a monoclonal antibody.

建立了采用多克隆或单克隆抗体和直接竞争酶联免疫吸附筛选法(ELISA)检测饲料中磺胺乙嗪(SMZ)污染的灵敏筛选方法。25.0 g饲料样品用0.5N HCl提取，离心。提取液用3.0N NaOH调至pH 7.0，再离心。该ph调整提取物用于ELISA。多克隆抗体在添加提取物中检测到低至0.004微克SMZ/g饲料;采用单克隆抗体检测饲料中0.4微克SMZ的含量。

引用次数: 0

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