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Enzymatic determination of free glutamic acid in dried soups and in minced sausages: NMKL collaborative study. 酶法测定干汤和碎香肠中游离谷氨酸:NMKL合作研究。
M T Hattula, H C Wallin

An enzymatic method for the determination of free glutamic acid in meat products and dried soups was collaboratively studied in 11 laboratories. In the presence of the enzyme glutamate dehydrogenase, L-glutamic acid is oxidatively deaminated by nicotinamide adenine dinucleotide (NAD) to 2-oxoglutarate. In a reaction catalyzed by diaphorase, the NADH thus formed converts 2-(p-iodophenyl)-3-(p-nitrophenyl)-5-phenyltetrazolium chloride to a formazan, which is measured in the visible range at 492 nm. Fourteen samples (7 samples of minced sausage and 7 samples of dried cauliflower soup) with glutamate contents varying between 0.4 and 16 g/kg were included in the study. Materials were distributed to participants as blind duplicates and as split level pairs. The mean relative standard deviation (RSDR) for reproducibility for the dried soup material containing glutamate between 7 and 16 g/kg was 4.6%. RSDR values for samples of minced sausage containing glutamate at lower levels (0.4-1.3 g/kg) were between 12 and 16%.

研究了肉制品和干汤中游离谷氨酸的酶法测定方法。在谷氨酸脱氢酶存在下,l -谷氨酸被烟酰胺腺嘌呤二核苷酸(NAD)氧化脱胺成2-氧葡萄糖酸酯。在diaphorase催化的反应中,由此形成的NADH将2-(对碘苯基)-3-(对硝基苯基)-5-苯基四氮唑氯转化为甲醛,其可见范围为492nm。14份样品(7份碎肠和7份干花椰菜汤)的谷氨酸含量在0.4 - 16 g/kg之间。材料以盲副本和分层对的形式分发给参与者。含谷氨酸7 ~ 16 g/kg的干汤料重复性的平均相对标准偏差(RSDR)为4.6%。含有较低水平谷氨酸(0.4-1.3 g/kg)的碎肠样品的RSDR值在12 - 16%之间。
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引用次数: 0
Analysis of trypsin inhibitors and lectins in white kidney beans (Phaseolus vulgaris, var. Processor) in a combined method. 联合方法分析白芸豆(Phaseolus vulgaris, var. Processor)中胰蛋白酶抑制剂和凝集素。
Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.940
J. Roozen, J. de Groot
Buffered saline extraction, affinity chromatography, and Folin-BSA protein assay were used consecutively to provide a combined method for analysis of trypsin inhibitors and lectins in white kidney beans (Phaseolus vulgaris, var. Processor). The method was tested by following the decrease of both antinutritional factors by germination of the beans for 7 days at 20 degrees C. Repeatability coefficients of variation were 2-7.4% for the trypsin inhibitors and 2.2-10% for the lectins. After 7 days of germination, trypsin inhibitors and lectins were reduced by 72 and 92%, respectively.
采用缓冲盐水萃取法、亲和层析法和Folin-BSA蛋白法,建立了白芸豆(Phaseolus vulgaris, var. Processor)中胰蛋白酶抑制剂和凝集素的联合分析方法。该方法通过在20℃条件下进行7 d的发芽试验,观察两种抗营养因子的降低情况,重复变异系数为胰蛋白酶抑制剂2-7.4%,凝集素2.2-10%。萌发7 d后,胰蛋白酶抑制剂和凝集素含量分别降低72%和92%。
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引用次数: 7
Polyvinyl chloride matrix membrane electrodes for manual and flow injection analysis of chloroquine in pharmaceutical preparations. 用于药物制剂中氯喹手工和流动注射分析的聚氯乙烯基质膜电极。
Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.900
S. Hassan, M. Ahmed
Two types of polyvinyl chloride (PVC) matrix membrane electrodes responsive to the antimalarial drug chloroquine have been constructed, electrochemically evaluated, compared and used in pharmaceutical analysis. Type 1 is the classic PVC model with chloroquine-tetraphenylborate (TPB) sensor; Type 2 is a coated silver disk without internal filling solution. Both electrode types exhibited rapid linear potentiometric response to the logarithmic concentration of diprotonated chloroquine cation in the 10(-1) - 10(-6)M range with calibration slopes 28-30 mV/concentration decade over the pH range 1.8-6.2. These electrodes were sensitive enough to permit determination of chloroquine phosphate at concentrations as low as 5 microgram/mL with good accuracy and precision. Determination of chloroquine in various pharmaceutical preparations using direct potentiometry and potentiometric titration with NaTPB gave an average recovery of 98.8% of the nominal values (SD 0.5%). The Type 2 electrode was also assessed in a flow-through sandwich cell for flow injection analysis. Results were compared with data obtained by the U.S. Pharmacopeia method.
构建了两种对抗疟药物氯喹有响应的聚氯乙烯(PVC)基质膜电极,并对其进行了电化学评价、比较,并将其用于药物分析。1型是带有氯喹-四苯基硼酸盐(TPB)传感器的经典PVC模型;类型2是没有内部填充溶液的涂层银盘。在10(-1)- 10(-6)M范围内,两种电极类型对双质子化氯喹阳离子的对数浓度均表现出快速的线性电位响应,在pH值1.8-6.2范围内,校准斜率为28-30 mV/浓度十年。这些电极足够灵敏,可以在低至5微克/毫升的浓度下测定磷酸氯喹,具有良好的准确性和精密度。采用直接电位法和硝酸甘油电位滴定法测定各种制剂中的氯喹,平均回收率为标称值的98.8% (SD为0.5%)。2型电极也在流动注射分析的流过夹层细胞中进行评估。结果与美国药典方法所得数据进行了比较。
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引用次数: 3
Liquid chromatographic determination of paraquat and diquat in crops using a silica column with aqueous ionic mobile phase. 水离子流动相硅柱液相色谱法测定作物中百草枯和双菊枯。
Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.961
T. M. Chichila, S. M. Walters
A method was developed for the determination of paraquat (PQ) and diquat (DQ) in high moisture food crops. Samples were digested with 6M HCl, and the herbicides were isolated from the digest using pH-controlled silica solid phase extraction. The analytes were then determined by ion-pairing liquid chromatography with a silica analytical column, sodium chloride as the ion-pairing reagent, and acetonitrile as the organic modifier. A diode array UV absorbance detector was used to simultaneously quantify PQ and DQ at their respective maximum absorbance wavelengths, 257 and 310 nm. Average recoveries of PQ and DQ standards from 4 different crops fortified at 0.01-0.50 ppm levels ranged from 79.3 to 104.8%.
建立了测定高水分粮食作物中百草枯(PQ)和双菊枯(DQ)含量的方法。样品用6M HCl消化,用ph控制的硅固相萃取法从消化物中分离除草剂。以二氧化硅分析柱,氯化钠为离子配对试剂,乙腈为有机改性剂,采用离子配对液相色谱法测定。采用二极管阵列紫外吸光度检测器,在最大吸光度波长257 nm和310 nm处同时定量PQ和DQ。在0.01 ~ 0.50 ppm强化条件下,4种不同作物的PQ和DQ标准的平均回收率为79.3 ~ 104.8%。
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引用次数: 14
Use of the Mycosep multifunctional cleanup column for liquid chromatographic determination of aflatoxins in agricultural products. 应用Mycosep多功能净化柱液相色谱法测定农产品中黄曲霉毒素。
Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.951
Thomas J Wilson, T. Romer
A liquid chromatographic (LC) technique has been developed that uses the Mycosep multifunctional cleanup (MFC) column. MFC columns provide a rapid 1-step extract purification. They are designed to retain particular groups of compounds that may create interferences in analytical methods. At the same time, MFC columns allow compounds of interest to pass through. In the method presented, test samples are extracted in a blender with acetonitrile-water (9 + 1). A portion of the extract is forced through an MFC column designed especially for analysis of numerous mycotoxins. Analytical interferences are retained, while aflatoxins pass through the column. Aflatoxins B1 and G1 are converted to their hemiacetals by heating a mixture of purified extract and water-trifluoroacetic acid-acetic acid (7 + 2 + 1) at 65 degrees C for 8.5 min. An aliquot of this mixture is analyzed by isocratic LC with acetonitrile-water mobile phase and fluorescence detection. A detection limit of less than 0.5 ng/g for aflatoxin B1 was obtained. Average recoveries greater than 95% total aflatoxins (B1, B2, G1, and G2) and coefficients of variation of less than 3% were obtained. The method was successfully applied to the following commodities: corn, almonds, pista-chios, walnuts, peanuts, Brazil nuts, milo, rice, cottonseed, corn meal, corn gluten meal, fig paste, and mixed feeds.
建立了一种使用Mycosep多功能清除(MFC)柱的液相色谱(LC)技术。MFC柱提供快速的一步萃取纯化。它们被设计用来保留可能对分析方法产生干扰的特定化合物群。同时,MFC柱允许感兴趣的化合物通过。在本文提出的方法中,测试样品在含有乙腈-水(9 + 1)的搅拌器中提取。一部分提取物强制通过专门为分析多种真菌毒素而设计的MFC柱。当黄曲霉毒素通过色谱柱时,分析干扰被保留。将纯化提取物与水-三氟乙酸-乙酸(7 + 2 + 1)的混合物在65℃加热8.5 min,将黄曲霉毒素B1和G1转化为半缩醛。该混合物的等温液相色谱采用乙腈-水流动相和荧光检测进行分析。黄曲霉毒素B1的检出限小于0.5 ng/g。黄曲霉毒素(B1、B2、G1和G2)的平均回收率大于95%,变异系数小于3%。该方法成功地应用于以下商品:玉米、杏仁、开心果、核桃、花生、巴西坚果、米米、大米、棉籽、玉米粉、玉米蛋白粉、无花果膏和混合饲料。
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引用次数: 50
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。
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: 0
Analysis of organochlorine pesticide residues using simultaneous injection of two capillary columns with electron capture and electrolytic conductivity detectors. 电子捕获电导检测器双毛细管柱同时进样分析有机氯农药残留。
Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.974
M. L. Hopper
A system has been developed that will allow low level screening of 31 organochlorine pesticide residues using simultaneous injection on 2 dissimilar capillary columns. An electron capture detector was attached to a DB-1701 column, and an electrolytic conductivity detector in the halogen mode was attached to a DB-5 column. Chlorinated pesticide amounts ranging from 0.05 ng for gamma-BHC to 1.5 ng for decamethrin can easily be quantitated and confirmed. The system can be used in either the column programmed mode or the isothermal column mode. Good reproducibility was obtained for injections in both modes. This system can easily be retrofitted to any gas chromatograph using on column or split/splitless injectors.
一个系统已开发,将允许低水平筛选31有机氯农药残留使用同时注射在两个不同的毛细管柱。电子捕获检测器连接在DB-1701柱上,卤素模式下的电解电导率检测器连接在DB-5柱上。氯化农药的量从γ -六六六的0.05 ng到十菊酯的1.5 ng都可以很容易地定量和确定。该系统既可用于柱程控模式,也可用于等温柱模式。在两种模式下均获得了良好的重现性。该系统可以很容易地改造到任何气相色谱仪使用柱或分裂/无分裂进样器。
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引用次数: 5
Liquid chromatographic determination of the processing aid 4-hexylresorcinol in shrimp. 虾中加工助剂4-己基间苯二酚的液相色谱测定。
Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.1003
J. M. King, A. J. Mcevily, R. Iyengar
A rapid, sensitive, liquid chromatographic (LC) method has been developed for determination of residuals of the processing aid, 4-hexylresorcinol, on shrimp meat. An aqueous homogenate of shrimp meat is extracted with ethyl acetate followed by precolumn preparation on a silica Sep-Pak cartridge. LC determination is preformed with a Nova-Pak C18 column, with UV detection at 214 nm. Sensitivity was 0.006 micrograms, and recovery from shrimp meat samples of known 4-hexylresorcinol addition was 94%. Shrimp treated with 4-hexylresorcinol under the recommended dip protocol had mean residuals of 1.18 ppm, with a standard deviation of 0.13 ppm.
建立了一种快速、灵敏的液相色谱法测定虾肉上加工助剂4-己基间苯二酚残留量的方法。用乙酸乙酯提取虾肉的水均质液,然后在硅胶Sep-Pak墨盒上进行柱前制备。色谱柱为Nova-Pak C18,紫外检测波长为214 nm。灵敏度为0.006微克,从已知添加4-己基间苯二酚的虾肉样品中回收率为94%。在推荐的浸出方案下,用4-己基间苯二酚处理的虾的平均残留量为1.18 ppm,标准差为0.13 ppm。
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引用次数: 14
Supercritical fluid extraction/enzyme assay: a novel technique to screen for pesticide residues in meat products. 超临界流体萃取/酶分析:一种筛选肉制品中农药残留的新技术。
Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.1013
J. E. France, J. King
The novel combination of supercritical fluid extraction (SFE) with an enzyme assay system has been used to screen meat products to detect the presence of pesticides. Analytes are collected in water by expanding supercritical carbon dioxide to atmospheric pressure through a restrictor and into an aqueous phase. The solution is then tested for the presence of pesticide residues by enzyme assay. Two experimental approaches have been used. Alachlor-fortified lard and bovine liver were monitored by static SFE coupled with an enzyme immunoassay. SFE of carbofuran-fortified frankfurters was coupled with an enzyme assay based on cholinesterase inhibition. A major benefit of the SFE/enzyme assay technique over conventional screening techniques is that the analyst is not exposed to organic solvents.
超临界流体萃取(SFE)与酶分析系统的新型组合已被用于筛选肉制品中农药的存在。分析物是通过节流器将超临界二氧化碳膨胀到大气压力并进入水相而在水中收集的。然后用酶测定法检测溶液中是否存在农药残留。采用了两种实验方法。采用静态SFE结合酶免疫分析法对甲氯草胺强化猪油和牛肝脏进行监测。对加了呋喃的法兰克福香肠进行了SFE测定,并结合了基于胆碱酯酶抑制的酶测定。与传统筛选技术相比,SFE/酶分析技术的一个主要优点是分析人员不暴露于有机溶剂中。
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引用次数: 7
Liquid chromatographic determination of paraquat and diquat in crops using a silica column with aqueous ionic mobile phase. 水离子流动相硅柱液相色谱法测定作物中百草枯和双菊枯。
T M Chichila, S M Walters

A method was developed for the determination of paraquat (PQ) and diquat (DQ) in high moisture food crops. Samples were digested with 6M HCl, and the herbicides were isolated from the digest using pH-controlled silica solid phase extraction. The analytes were then determined by ion-pairing liquid chromatography with a silica analytical column, sodium chloride as the ion-pairing reagent, and acetonitrile as the organic modifier. A diode array UV absorbance detector was used to simultaneously quantify PQ and DQ at their respective maximum absorbance wavelengths, 257 and 310 nm. Average recoveries of PQ and DQ standards from 4 different crops fortified at 0.01-0.50 ppm levels ranged from 79.3 to 104.8%.

建立了测定高水分粮食作物中百草枯(PQ)和双菊枯(DQ)含量的方法。样品用6M HCl消化,用ph控制的硅固相萃取法从消化物中分离除草剂。以二氧化硅分析柱,氯化钠为离子配对试剂,乙腈为有机改性剂,采用离子配对液相色谱法测定。采用二极管阵列紫外吸光度检测器,在最大吸光度波长257 nm和310 nm处同时定量PQ和DQ。在0.01 ~ 0.50 ppm强化条件下,4种不同作物的PQ和DQ标准的平均回收率为79.3 ~ 104.8%。
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引用次数: 0
期刊
Journal - Association of Official Analytical Chemists
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