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A new approach to the study of glucosinolates by isocratic liquid chromatography. Part I. Rapid determination of desulfated derivatives of rapeseed glucosinolates. 等密度液相色谱法研究硫代葡萄糖苷的新方法。第一部分快速测定油菜籽硫代葡萄糖苷的脱硫衍生物。
A Quinsac, D Ribaillier, C Elfakir, M Lafosse, M Dreux

Liquid chromatographic (LC) analysis of desulfated derivatives of rapeseed glucosinolates has been carried out under isocratic elution conditions with different CN-bonded stationary phases. The effects of the eluant composition (water, acetonitrile, and methanol) with the stationary phase (Zorbax CN, Lichrospher CN, and Ultrasphere CN) and temperature (20 and 50 degrees C) are described. An isocratic LC method performed at room temperature using a Lichrospher CN column and water as mobile phase is proposed. The chromatographic analysis can be done in less than 12 min, and it is easier and less expensive than the traditional gradient mode. Four commercial samples of rapeseed containing various quantities of other cruciferous seeds (wild mustard and stinkweed) as an admixture have been analyzed to determine the total glucosinolate content. Relative standard deviations of repeatability of the isocratic and gradient LC methods ranged from 0.4 to 1.7% and from 2.7 to 4.7%, respectively. Comparison of the results showed good agreement between the 2 methods (beter than 98%).

采用不同的cn键固定相,在等密度洗脱条件下对油菜籽硫代葡萄糖苷衍生物进行了液相色谱分析。描述了洗脱液组成(水、乙腈和甲醇)与固定相(Zorbax CN、Lichrospher CN和Ultrasphere CN)和温度(20和50℃)的影响。提出了一种在室温下以利氏CN柱和水为流动相的等压液相色谱法。色谱分析可在12分钟内完成,比传统的梯度模式更简单,成本更低。四个商业油菜籽样品含有不同数量的其他十字花科种子(野生芥菜和臭草)作为混合物,以确定总硫代葡萄糖苷的含量。等距色谱法和梯度色谱法重复性的相对标准偏差分别为0.4 ~ 1.7%和2.7 ~ 4.7%。结果表明,两种方法吻合度均在98%以上。
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引用次数: 0
Limited survey of residual tetracyclines in tissues collected from diseased animals in Aichi Prefecture, Japan. 日本爱知县患病动物组织中残留四环素的有限调查。
Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.894
H. Oka, Y. Ikai, N. Kawamura, J. Hayakawa
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.
收集组织调查日本爱知县屠宰场因出现疾病症状而未通过检验的屠宰动物体内四环素类抗生素残留的实际情况。用液相色谱法对组织进行分析。271份样品中土霉素(OTC)阳性49份(18.1%),金霉素(CTC)阳性5份(1.8%),强力霉素(DC)阳性5份(1.8%)。一个样本(牛肾)OTC和DC均呈阳性。但未检出四环素。牛和猪的TCs残留频率分别为29.1%(37/127)和15.2%(22/144)。肾脏样本的TCs残留发生率较高,其残留浓度是肝脏和其他样本的1.5-7倍。
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引用次数: 7
Potassium as an index of fruit content in baby food products. Part I. Banana-containing and apricot-containing products. 钾作为婴儿食品中水果含量的指标。第一部分:含香蕉和含杏的产品。
Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.929
R. Harvey, R. Theuer
Percentage ingredient labeling has been proposed for baby foods. We determined whether or not the potassium content of baby foods could be used to verify the quantity of fruit when the characterizing ingredients were apricots or bananas, fruits rich in potassium. Official values for potassium in fruit (USDA Handbook No. 8-9) did not agree well with actual analyses. The potassium levels of products of known composition were accurately predicted from analyses of the actual ingredients used to make the foods. For banana-containing monofruit products of variable or unknown composition, potassium analysis led to fruit level estimates consistent with either the known composition or the label declaration. For products of unknown composition made with apricot concentrate, however, potassium analysis led to fruit level estimates lower than the probable fruit content. The quantity of fruit in baby foods made with potassium-rich fruits can be estimated from the potassium content if the potassium value for the fruit is representative of the actual ingredients used to make the product. If potassium analysis is to be used to verify compliance with percentage ingredient labeling, there must be statutory specification of the single-strength fruit level for fruit reconstituted from concentrate.
有人提议在婴儿食品上标注成分百分比。我们确定婴儿食品的钾含量是否可以用来验证水果的数量,当特征成分是杏或香蕉,富含钾的水果。水果中钾的官方值(美国农业部手册第8-9号)与实际分析不太一致。已知成分产品的钾含量是通过分析制作食品的实际成分准确预测出来的。对于含有可变或未知成分的香蕉单果产品,钾分析得出的水果水平估计与已知成分或标签声明一致。然而,对于用杏浓缩液制成的成分未知的产品,钾分析导致果实水平估价值低于可能的果实含量。用富含钾的水果制成的婴儿食品中的水果含量可以通过钾含量来估计,如果水果的钾值代表了制作该产品所使用的实际成分。如果钾分析是用来验证符合百分比成分标签,必须有单一强度的水果水平的法定规格,从浓缩物中重组的水果。
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引用次数: 2
Potassium as an index of fruit content in baby food products. Part I. Banana-containing and apricot-containing products. 钾作为婴儿食品中水果含量的指标。第一部分:含香蕉和含杏的产品。
R A Harvey, R C Theuer

Percentage ingredient labeling has been proposed for baby foods. We determined whether or not the potassium content of baby foods could be used to verify the quantity of fruit when the characterizing ingredients were apricots or bananas, fruits rich in potassium. Official values for potassium in fruit (USDA Handbook No. 8-9) did not agree well with actual analyses. The potassium levels of products of known composition were accurately predicted from analyses of the actual ingredients used to make the foods. For banana-containing monofruit products of variable or unknown composition, potassium analysis led to fruit level estimates consistent with either the known composition or the label declaration. For products of unknown composition made with apricot concentrate, however, potassium analysis led to fruit level estimates lower than the probable fruit content. The quantity of fruit in baby foods made with potassium-rich fruits can be estimated from the potassium content if the potassium value for the fruit is representative of the actual ingredients used to make the product. If potassium analysis is to be used to verify compliance with percentage ingredient labeling, there must be statutory specification of the single-strength fruit level for fruit reconstituted from concentrate.

有人提议在婴儿食品上标注成分百分比。我们确定婴儿食品的钾含量是否可以用来验证水果的数量,当特征成分是杏或香蕉,富含钾的水果。水果中钾的官方值(美国农业部手册第8-9号)与实际分析不太一致。已知成分产品的钾含量是通过分析制作食品的实际成分准确预测出来的。对于含有可变或未知成分的香蕉单果产品,钾分析得出的水果水平估计与已知成分或标签声明一致。然而,对于用杏浓缩液制成的成分未知的产品,钾分析导致果实水平估价值低于可能的果实含量。用富含钾的水果制成的婴儿食品中的水果含量可以通过钾含量来估计,如果水果的钾值代表了制作该产品所使用的实际成分。如果钾分析是用来验证符合百分比成分标签,必须有单一强度的水果水平的法定规格,从浓缩物中重组的水果。
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引用次数: 0
Monitoring aldehyde production during frying by reversed-phase liquid chromatography. 反相液相色谱法监测煎炸过程中醛的生成。
Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.957
Ralph H Lane, Janis L Smathers
Acrolein (2-propenal) and other low molecular weight aldehydes (LMWAs) formed by degradation of the frying medium (triglycerides) were monitored by liquid chromatography (LC) during preparation of fried items. LMWA contents of coatings from codfish and of doughnuts and their volatiles that codistill with steam are monitored by trapping the vapors and distillate from the food matrix in a 2,4-dinitrophenylhydrazine solution. The resulting hydrazones are partitioned from the aqueous phase, first into isooctane and then into acetonitrile for LC analysis. The hydrazones are separated and quantified on a C18 reversed-phase column with acetonitrile-water as the mobile phase. LMWAs are confirmed by gas chromatography/mass spectrometry. No difference was found in LMWA content in coatings from fish fillets fried at 182 or 204 degrees C. Cake doughnuts were higher in acrolein content than yeast-raised doughnuts prepared under similar conditions. Freshness of the frying medium, frying time, and batch size did not seem to influence LMWA production from doughnuts. Results indicated that most of the LMWAs formed codistilled with steam during frying rather than remaining with the food item.
采用液相色谱法(LC)对制备油炸食品过程中由油炸介质(甘油三酯)降解形成的丙烯醛(2-propenal)和其他低分子量醛(LMWAs)进行了监测。用蒸汽蒸馏的鳕鱼和甜甜圈的涂层及其挥发物的低分子苯胺含量是通过捕获蒸汽和从2,4-二硝基苯肼溶液中从食物母体中蒸馏出来来监测的。得到的腙从水相分离,首先进入异辛烷,然后进入乙腈进行LC分析。在C18反相色谱柱上,以乙腈-水为流动相分离和定量。LMWAs通过气相色谱/质谱法证实。在182℃和204℃下煎炸的鱼片涂层的低分子纤维素含量没有差异,蛋糕甜甜圈的丙烯醛含量高于在相同条件下制作的酵母发酵甜甜圈。油炸介质的新鲜度、油炸时间和批量大小似乎不影响从甜甜圈生产低分子微波。结果表明,在油炸过程中,大部分LMWAs与蒸汽共蒸馏形成,而不是留在食品中。
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引用次数: 17
Assay of oxolinic acid residues in salmon muscle by liquid chromatography with fluorescence detection: interlaboratory study. 荧光液相色谱法测定鲑鱼肌肉中氧喹啉酸残留量:实验室间研究。
Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.906
G. Carignan, L. Larocque, S. Sved
A previously developed method that uses a simplified sample preparation and fluorometric detection of liquid chromatographic eluates for the determination of oxolinic acid in salmon muscle has been collaboratively studied. Five laboratories participated in the study to analyze, in quintuplicate, blank salmon muscle fortified at 10, 20, 50, and 100 micrograms/kg (ppb), and 2 incurred samples from salmon given feed with medicated oxolinic acid. The tissue, 2 g mixed with 2 g Na2SO4, is extracted with ethyl acetate and centrifuged, and the solvent is evaporated. The residue is partitioned in a mixture of hexane and 0.01 M oxalic acid, and the aqueous phase is chromatographed using fluorescence detection at 327 nm excitation and 369 nm emission. Mean recoveries ranged from 77.2 to 84.5% in spiked samples with reproducibility relative standard deviation (RSDR) ranging from 11.5 to 18.3%. Treated salmon were found to contain 8.71 and 53.8 micrograms/kg with RSDR of 18.6 and 16.7%, respectively. The corresponding repeatability relative standard deviations (RSDR) were 5.8-12.2%, and 7.7 and 6.2%. The method is recommended for regulatory purposes in Canada.
合作研究了先前开发的一种方法,该方法使用简化的样品制备和液相色谱洗脱液的荧光检测来测定鲑鱼肌肉中的氧喹啉酸。五个实验室参与了这项研究,分五次分析了添加了10、20、50和100微克/公斤(ppb)的空白鲑鱼肌肉,两个实验室从喂食了药物氧喹啉酸的鲑鱼中提取了样本。将组织与2g Na2SO4混合,用乙酸乙酯提取,离心,蒸发溶剂。残渣在正己烷和0.01 M草酸的混合物中分离,在327 nm激发和369 nm发射的荧光检测下进行水相色谱。加标样品的平均回收率为77.2 ~ 84.5%,重现性相对标准偏差(RSDR)为11.5 ~ 18.3%。经处理的三文鱼含8.71和53.8微克/公斤,RSDR分别为18.6%和16.7%。相应的重复性相对标准偏差(RSDR)分别为5.8 ~ 12.2%、7.7、6.2%。该方法被推荐用于加拿大的监管目的。
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引用次数: 4
A new approach to the study of glucosinolates by isocratic liquid chromatography. Part I. Rapid determination of desulfated derivatives of rapeseed glucosinolates. 等密度液相色谱法研究硫代葡萄糖苷的新方法。第一部分快速测定油菜籽硫代葡萄糖苷的脱硫衍生物。
Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.932
A. Quinsac, D. Ribaillier, C. Elfakir, M. Lafosse, M. Dreux
Liquid chromatographic (LC) analysis of desulfated derivatives of rapeseed glucosinolates has been carried out under isocratic elution conditions with different CN-bonded stationary phases. The effects of the eluant composition (water, acetonitrile, and methanol) with the stationary phase (Zorbax CN, Lichrospher CN, and Ultrasphere CN) and temperature (20 and 50 degrees C) are described. An isocratic LC method performed at room temperature using a Lichrospher CN column and water as mobile phase is proposed. The chromatographic analysis can be done in less than 12 min, and it is easier and less expensive than the traditional gradient mode. Four commercial samples of rapeseed containing various quantities of other cruciferous seeds (wild mustard and stinkweed) as an admixture have been analyzed to determine the total glucosinolate content. Relative standard deviations of repeatability of the isocratic and gradient LC methods ranged from 0.4 to 1.7% and from 2.7 to 4.7%, respectively. Comparison of the results showed good agreement between the 2 methods (beter than 98%).
采用不同的cn键固定相,在等密度洗脱条件下对油菜籽硫代葡萄糖苷衍生物进行了液相色谱分析。描述了洗脱液组成(水、乙腈和甲醇)与固定相(Zorbax CN、Lichrospher CN和Ultrasphere CN)和温度(20和50℃)的影响。提出了一种在室温下以利氏CN柱和水为流动相的等压液相色谱法。色谱分析可在12分钟内完成,比传统的梯度模式更简单,成本更低。四个商业油菜籽样品含有不同数量的其他十字花科种子(野生芥菜和臭草)作为混合物,以确定总硫代葡萄糖苷的含量。等距色谱法和梯度色谱法重复性的相对标准偏差分别为0.4 ~ 1.7%和2.7 ~ 4.7%。结果表明,两种方法吻合度均在98%以上。
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引用次数: 10
Comparison of automated liquid chromatographic and bioassay methods for determining spiramycin concentration in bovine plasma. 自动液相色谱法和生物测定法测定牛血浆中螺旋霉素浓度的比较。
Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.912
P. Sanders, G. Moulin, C. Gaudiche, B. Delepine, D. Mourot
The performance of a liquid chromatographic (LC) method for spiramycin measurement in bovine plasma has been compared with that of a microbiological method. Plasma samples were obtained from cattle administered spiramycin intravenously. Comparison tests used were intraclass correlation (r1), correlation (r), and Student's paired t-test. For concentrations lower than 2.5 IU/mL, microbiological values were higher than LC values. This difference in results modified pharmacokinetic interpretation and might be explained by the presence of microbiologically active metabolites.
本文比较了液相色谱法和微生物法测定牛血浆中螺旋霉素的性能。从静脉注射螺旋霉素的牛身上获得血浆样本。比较检验采用类内相关性(r1)、相关性(r)和学生配对t检验。浓度低于2.5 IU/mL时,微生物学值高于LC值。这种结果的差异修改了药代动力学的解释,可能是由于存在微生物活性代谢物。
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引用次数: 2
Monitoring aldehyde production during frying by reversed-phase liquid chromatography. 反相液相色谱法监测煎炸过程中醛的生成。
R H Lane, J L Smathers

Acrolein (2-propenal) and other low molecular weight aldehydes (LMWAs) formed by degradation of the frying medium (triglycerides) were monitored by liquid chromatography (LC) during preparation of fried items. LMWA contents of coatings from codfish and of doughnuts and their volatiles that codistill with steam are monitored by trapping the vapors and distillate from the food matrix in a 2,4-dinitrophenylhydrazine solution. The resulting hydrazones are partitioned from the aqueous phase, first into isooctane and then into acetonitrile for LC analysis. The hydrazones are separated and quantified on a C18 reversed-phase column with acetonitrile-water as the mobile phase. LMWAs are confirmed by gas chromatography/mass spectrometry. No difference was found in LMWA content in coatings from fish fillets fried at 182 or 204 degrees C. Cake doughnuts were higher in acrolein content than yeast-raised doughnuts prepared under similar conditions. Freshness of the frying medium, frying time, and batch size did not seem to influence LMWA production from doughnuts. Results indicated that most of the LMWAs formed codistilled with steam during frying rather than remaining with the food item.

采用液相色谱法(LC)对制备油炸食品过程中由油炸介质(甘油三酯)降解形成的丙烯醛(2-propenal)和其他低分子量醛(LMWAs)进行了监测。用蒸汽蒸馏的鳕鱼和甜甜圈的涂层及其挥发物的低分子苯胺含量是通过捕获蒸汽和从2,4-二硝基苯肼溶液中从食物母体中蒸馏出来来监测的。得到的腙从水相分离,首先进入异辛烷,然后进入乙腈进行LC分析。在C18反相色谱柱上,以乙腈-水为流动相分离和定量。LMWAs通过气相色谱/质谱法证实。在182℃和204℃下煎炸的鱼片涂层的低分子纤维素含量没有差异,蛋糕甜甜圈的丙烯醛含量高于在相同条件下制作的酵母发酵甜甜圈。油炸介质的新鲜度、油炸时间和批量大小似乎不影响从甜甜圈生产低分子微波。结果表明,在油炸过程中,大部分LMWAs与蒸汽共蒸馏形成,而不是留在食品中。
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引用次数: 0
Improved method for determination of polynuclear aromatic hydrocarbons in pharmacopoeial paraffin and mineral oils. 药典石蜡和矿物油中多核芳烃测定方法的改进。
A Geahchan, I Le Gren, P Chambon, R Chambon

An improved method has been developed for quantitative determination of polynuclear aromatic hydrocarbons (PAHs) in pharmacopoeial paraffin and medicinal white oil samples. This new method combines 2 liquid-liquid partition and adsorption chromatography procedures with a 2-step purification on Sephadex LH 20 and liquid chromatography with fluorometric determination. Selective elution of PAHs results in absence of background fluorescence. The minimum detectable level ranges from 0.2 ppt for benzofluoranthene isomers to 200 ppt for acenaphthene. Recoveries of PAHs added at 7 ppm varied from 92.1 to 111.4%. When a variety of medicinal white oil samples were analyzed by this improved method, 27 PAHs were identified, including 11 suspected carcinogens. Their identities were confirmed by capillary gas chromatography.

建立了药典石蜡和药用白油样品中多核芳烃(PAHs)的定量测定方法。该方法结合了液液分离和吸附色谱两步法,在Sephadex LH 20上进行两步纯化,并结合了液相色谱法和荧光法测定。选择性洗脱多环芳烃导致没有背景荧光。最低可检测水平从苯并氟蒽异构体的0.2 ppt到苊的200 ppt不等。添加7 ppm时,多环芳烃的回收率从92.1%到111.4%不等。对多种药用白油样品进行分析,鉴定出27种多环芳烃,其中疑似致癌物11种。用毛细管气相色谱法对其进行了鉴定。
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引用次数: 0
期刊
Journal - Association of Official Analytical Chemists
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