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Quantitative Analysis of Daidzin, Daidzein, Genistin and Genistein in Various Foods by HPLC 高效液相色谱法定量分析各种食品中的大豆苷元、大豆苷元、染料木素和染料木素
Pub Date : 1999-12-05 DOI: 10.3358/SHOKUEISHI.40.6_444
Y. Kikuchi, Y. Shimamura, M. Hirokado, K. Yasuda, M. Nishijima
A method was developed for the separation and analysis of isoflavone β-glycoside conjugates (daidzin, genistin) and aglucones (daidzein, genistein) in various foods.The isoflavones were extracted from dried samples with 80% aqueous methanol and from aqueous samples with methanol, and analyzed by reversed-phase HPLC using a gradient of methanol-water as the eluent.The recoveries of four kinds of isoflavones added to various foods were in the range of 84-104%. The limit of detection was 0.1μg/g in samples.Using the proposed method, 205 samples of commercial foods and other products were analyzed. Large amounts of isoflavones were detected mainly in soybeans and soy products. For example, in dry soybean seeds (n=12), daidzin was at the level of 270-1, 100μg/g, daidzein at 20-270μg/g, genistin at 370-1, 200μg/g and genistein at 21-350μg/g.
建立了一种分离分析各种食品中异黄酮β-糖苷偶联物(大豆苷元、染料木素)和聚糖素(大豆苷元、染料木素)的方法。分别用80%甲醇水溶液和甲醇水溶液提取干燥样品中的异黄酮,用甲醇-水梯度反相高效液相色谱法进行分析。添加到不同食品中的4种异黄酮的加样回收率在84 ~ 104%之间。样品的检出限为0.1μg/g。利用该方法对205份商品食品和其他产品样品进行了分析。在大豆和豆制品中检测到大量异黄酮。例如,在干大豆种子(n=12)中,大豆黄酮含量为270 ~ 1,100 μg/g,大豆黄酮含量为20 ~ 270μg/g,染料木素含量为370 ~ 1,200 μg/g,染料木素含量为21 ~ 350μg/g。
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引用次数: 4
Food-borne Infection Induced by the Consumption of Salad Vegetables and Fruits 食用沙拉蔬菜和水果引起的食源性感染
Pub Date : 1999-12-05 DOI: 10.3358/SHOKUEISHI.40.6_417
K. Kaneko
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引用次数: 2
Analysis of β-Carotene and Paprika Color in Foods Using Reversed-phase Thin-layer Chromatography/Scanning Densitometry 反相薄层色谱/扫描密度法分析食品中β-胡萝卜素和红辣椒的颜色
Pub Date : 1999-10-05 DOI: 10.3358/SHOKUEISHI.40.5_356
Tomoko Hayashi, E. Ueno, Yuko Ito, H. Oka, N. Ozeki, Y. Itakura, S. Yamada, T. Kagami, Atsuo Kajita, J. Fujita, Masao Ono
A technique for the analysis of β-carotene and paprika color in foods using reversed-phase TLC and scanning densitometry was established. Both colors were extracted with ethyl ether from foods. Extract of β-carotene was directly cleaned up with a C18 cartridge and extract of paprika color was cleaned up with a C18 cartridge after saponification with 5% sodium hydroxide in methanol. Separation of both extracts was achieved on the reversed-phase C18 TLC plate using acetonitrile-acetone-n-hexane (11:7:2) as the solvent system. The visible absorption spectra of the extracts were measured using scanning densitometry without isolation of the colors. In order to investigate the capability of the present method, 77 commercial foods were analyzed, and their chromatographic behaviors and spectra were observed. The separation and the spectra obtained were not affected by coexisting substances in the foods and the spots always gave the same Rf values and spectra as the standards, with good reproducibility. The present method is considered to be useful for the rapid analysis of β-carotene and paprika color in foods.
建立了反相薄层色谱和扫描密度法分析食品中β-胡萝卜素和红辣椒颜色的方法。这两种颜色都是用乙醚从食物中提取的。β-胡萝卜素提取液直接用C18滤筒清洗,辣椒色提取液用5%氢氧化钠在甲醇中皂化后用C18滤筒清洗。在反相C18薄层色谱板上,以乙腈-丙酮-正己烷(11:7:2)为溶剂体系对两种提取物进行分离。在不分离颜色的情况下,用扫描密度法测定了提取物的可见吸收光谱。为了验证该方法的有效性,对77种商品食品进行了分析,并对其色谱行为和光谱进行了观察。得到的分离和光谱不受食品中共存物质的影响,斑点的Rf值和光谱与标准值一致,重现性好。本方法可用于食品中β-胡萝卜素和红辣椒颜色的快速分析。
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引用次数: 6
Simple and Rapid Analysis of Penicillins in Milk by HPLC Using Multidimensional: On-line Clean-up and Post-column Photolysis with UV Detection 多维在线净化-柱后光解-紫外检测高效液相色谱法简单快速分析牛奶中青霉素
Pub Date : 1999-10-05 DOI: 10.3358/SHOKUEISHI.40.5_375
S. Taguchi, S. Yoshida, Yukio Tanaka, S. Hori
The method was established by using C18 solid-phase extraction, on-line clean-up and post-column photochemical derivatization HPLC with UV detection at 310nm. Penicillins, having UV absorption maxima less than 230nm, were converted quantitatively to molecules having 310nm absorption maxima by photochemical degration. Recoveries at a level of 0.004mg/L were in the range from 87 to 110%. The quantitation limit was 0.002 for penicillin G, oxacillin, cloxacillin and dicloxacillin and 0.004mg/L for nafcillin.
采用C18固相萃取、在线净化、柱后光化学衍生化高效液相色谱(HPLC)和紫外检测(310nm)建立了该方法。通过光化学降解,将最大紫外吸收小于230nm的青霉素定量转化为最大紫外吸收310nm的分子。在0.004mg/L的加样回收率为87% ~ 110%。青霉素G、奥西林、氯西林、双氯西林的定量限为0.002 mg/L,萘西林的定量限为0.004mg/L。
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引用次数: 11
Toxicity and Tetrodotoxin as the Toxic Principle of a Brackish Water Puffer, Tetraodon steindachneri, Collected from Thailand 泰国半咸淡水河豚的毒性和河豚毒素的毒性原理
Pub Date : 1999-10-05 DOI: 10.3358/SHOKUEISHI.40.5_391
Y. Mahmud, K. Yamamori, T. Noguchi
A total of 399 specimens of a brackish water puffer, Tetraodon steindachneri, were collected from Thailand during February 1997 to September 1998, and assayed for their toxicity by mouse test. The highest lethal potency was found in skin followed by muscle, intestine and gonad. The puffers which were reared in an aquarium showed lower toxicity than those monitored immediately after collection. The toxin was partially purified by ultrafiltration using a YM-1 membrane and several types of chromatography, activated charcoal, Bio-Gel P-2 and Bio-Rex 70. The toxin was characterized as tetrodotoxin (TTX) on the basis of electrophoresis, HPLC, LC/MS and 1H-NMR analyses.
1997年2月至1998年9月期间,我们在泰国共采集了399只淡咸水河豚(Tetraodon steindachneri)标本,并进行了小鼠毒性试验。致死性最强的部位是皮肤,其次是肌肉、肠道和性腺。在水族箱中饲养的河豚的毒性低于收集后立即监测的河豚。采用m -1膜和几种色谱、活性炭、Bio-Gel P-2和Bio-Rex 70进行超滤,部分纯化毒素。通过电泳、HPLC、LC/MS和1H-NMR分析,鉴定该毒素为河豚毒素(TTX)。
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引用次数: 18
Occurrence of TTX in a Brackish Water Puffer “Midorifugu”, Tetraodon nigroviridis, Collected from Thailand 泰国淡淡水河豚“米多里河豚”中TTX的发生
Pub Date : 1999-10-05 DOI: 10.3358/SHOKUEISHI.40.5_363
Y. Mahmud, K. Yamamori, T. Noguchi
Screening tests were carried out on the toxicity of a brackish water puffer, Tetraodon nigroviridis, collected from Thailand through November, 1996 to May, 1998. Among the different tissues, the skin showed the highest toxicity scores, ranging from 49.2-286MU/g, followed by muscle (5.4-11MU/g), while liver and intestine mostly gave scores under 5MU/g. The toxin was partially purified by three kinds of column chromatography consisting of activated charcoal, Bio-Gel P-2 and Bio-Rex 70. Analyses by HPLC, TLC, electrophoresis, 1H-NMR and LC/MS identified the purified toxin as tetrodotoxin.
1996年11月至1998年5月期间,对在泰国收集的一种咸淡水河豚——黑病毒四齿鲨的毒性进行了筛选试验。在不同组织中,皮肤的毒性评分最高,在49.2-286MU/g之间,其次是肌肉(5.4-11MU/g),而肝脏和肠道的毒性评分大多在5MU/g以下。采用活性炭、Bio-Gel P-2和Bio-Rex 70三种色谱柱对毒素进行部分纯化。经HPLC、TLC、电泳、1H-NMR和LC/MS分析,鉴定为河豚毒素。
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引用次数: 37
Effect of Methanol Extract from Fruit Body of Mycoleptodonoides aitchisonii on Acute and Chronic Inflammation Models 青衣霉霉子实体甲醇提取物对急慢性炎症模型的影响
Pub Date : 1999-10-05 DOI: 10.3358/SHOKUEISHI.40.5_368
Y. Kasahara, K. Yasukawa, K. Kumaki
We have been investigating biological activities of components of natural foods. In this study, we found an antiinflammatory effect of edible mushroom, Micoleptodonoides aitchisonii (bunaharitake: Japanese name), on oral administration in mouse and rat acute and chronic inflammation models. M. aitchisonii extract significantly suppressed hind-paw edema induced by carrageenin. Furthermore, the extract not only inhibited the hind-paw edema induced by various acute phlogists such as histamine, serotonin, bradikinin, prostaglandin E1, but also suppressed the increase of vascular permeability induced by acetic acid, indicating that it primarily acts at the exudative stage of inflammation.M. aitchisonii extract inhibited both the proliferation of granulation tissue tested by a cotton pellet method and a development of adjuvant arthritis in rats, demonstrating that the extract might be effective against chronic inflammation.
我们一直在研究天然食品成分的生物活性。在本研究中,我们发现食用菌Micoleptodonoides aitchisonii(日本名:bunaharitake)对小鼠和大鼠急性和慢性炎症模型具有抗炎作用。青藤提取物对角叉菜胶致后爪水肿有显著抑制作用。此外,该提取物不仅能抑制组胺、血清素、缓动素、前列腺素E1等多种急性炎症诱导的后爪水肿,还能抑制醋酸诱导的血管通透性增加,表明其主要作用于炎症的渗出期。黄芩提取物对棉球法试验的肉芽组织增殖和大鼠佐剂性关节炎的发展均有抑制作用,表明黄芩提取物可能对慢性炎症有效。
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引用次数: 0
Study on GC/MS (SIM) for Determination of Carbamate and Organonitrogen Pesticides in Foods with Simple Clean-up by SPE Method 气相色谱/质谱法测定食品中氨基甲酸酯和有机氮农药的研究
Pub Date : 1999-10-05 DOI: 10.3358/SHOKUEISHI.40.5_382
M. Kawasaki, Tsuyoshi Inoue, K. Fukuhara, S. Uchiyama
Studies to develop a GC/MS (SIM) method for the determination of 34 pesticides including carbamates and organonitrogen pesticides in foods with solid-phase extraction (SPE) were conducted.Three kinds of SPE columns, a porous diatomaceous earth cartridge column, a diatomite column with a mini C18 cartridge column and a Florisil cartridge column were used successively to clean-up the extract from foods as an alternative to a separatory funnel for liquid-liquid partition. The handling was simpler than the conventional method and gave high recoveries of the pesticides.In GC/MS (SIM), 2 to 4 different fragment ions were selected for each pesticide so that the GC/MS (SIM) identification could be done more accurately for multi-residue analysis of carbamate and organonitrogen pesticides. This simpler method was applicable for 29 pesticides out of 34 with almost the same recoveries and detection limits as the conventional method.
建立了固相萃取(SPE)法测定食品中氨基甲酸酯类、有机氮类等34种农药的GC/MS (SIM)方法。分别采用多孔硅藻土柱、硅藻土柱带微型C18柱和Florisil柱3种固相萃取柱对食品提取物进行净化,替代分离漏斗进行液液分离。该方法操作简便,农药回收率高。在GC/MS (SIM)中,每种农药选择2 ~ 4个不同的片段离子,以便更准确地进行氨基甲酸酯类和有机氮类农药的多残留分析。该法适用于34种农药中的29种,回收率和检出限与常规方法基本相同。
{"title":"Study on GC/MS (SIM) for Determination of Carbamate and Organonitrogen Pesticides in Foods with Simple Clean-up by SPE Method","authors":"M. Kawasaki, Tsuyoshi Inoue, K. Fukuhara, S. Uchiyama","doi":"10.3358/SHOKUEISHI.40.5_382","DOIUrl":"https://doi.org/10.3358/SHOKUEISHI.40.5_382","url":null,"abstract":"Studies to develop a GC/MS (SIM) method for the determination of 34 pesticides including carbamates and organonitrogen pesticides in foods with solid-phase extraction (SPE) were conducted.Three kinds of SPE columns, a porous diatomaceous earth cartridge column, a diatomite column with a mini C18 cartridge column and a Florisil cartridge column were used successively to clean-up the extract from foods as an alternative to a separatory funnel for liquid-liquid partition. The handling was simpler than the conventional method and gave high recoveries of the pesticides.In GC/MS (SIM), 2 to 4 different fragment ions were selected for each pesticide so that the GC/MS (SIM) identification could be done more accurately for multi-residue analysis of carbamate and organonitrogen pesticides. This simpler method was applicable for 29 pesticides out of 34 with almost the same recoveries and detection limits as the conventional method.","PeriodicalId":17269,"journal":{"name":"Journal of The Food Hygienic Society of Japan (shokuhin Eiseigaku Zasshi)","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1999-10-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89782913","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 3
Determination of Spiramycin I and Its Primary Metabolite Neospiramycin I in Meat, Milk and Fish by HPLC 高效液相色谱法测定肉、奶、鱼中螺旋霉素及其初级代谢物新螺旋霉素的含量
Pub Date : 1999-10-05 DOI: 10.3358/SHOKUEISHI.40.5_401
M. Horie, Y. Kido, M. Murayama, M. Toyoda, H. Nakazawa
A simple and rapid method using HPLC for the determination of spiramycin I (major and most important component) and its metabolite, neospiramycin I, in meat, fish and milk has been developed. Neospiramycin I was obtained by acidic treatment of spiramycin I. The drugs were extracted with 1.2% metaphosphoric acid-methanol (5:5), and the extracts were cleaned up on a Bond Elut SCX (500mg) cartridge. The HPLC separation was performed on a Puresil 5C18 column (150×4.6mm i. d.) using 0.05mol/L phosphate buffer (pH 2.5) -acetonitrile (76:24) as the mobile phase at a flow rate of 0.5mL/min. The drugs were detected at 235nm. The calibration graphs were rectilinear from 2 to 50ng for both drugs. The recoveries of the drugs from meat, milk and fish at the level of 0.2μg/g were 80.3-85.3%, and detection limits were 0.05μg/g for both drugs.
建立了高效液相色谱法测定肉类、鱼类和牛奶中螺旋霉素I(主要和最重要的成分)及其代谢物新螺旋霉素I的简便、快速方法。用1.2%偏磷酸-甲醇(5:5)提取药物,用Bond Elut SCX (500mg)药筒清洗。色谱柱为Puresil 5C18 (150×4.6mm),流动相为0.05mol/L磷酸缓冲液(pH 2.5) -乙腈(76:24),流速为0.5mL/min。药物在235nm处检测。两种药物的校准图在2 ~ 50ng范围内呈直线关系。在0.2μg/g水平下,三种药物的回收率为80.3 ~ 85.3%,两种药物的检出限均为0.05μg/g。
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引用次数: 5
Determination of Erythromycin and Oleandomycin in Meat and Fish by LC/MS 液相色谱/质谱法测定肉类和鱼类中红霉素和夹竹桃霉素的含量
Pub Date : 1999-08-05 DOI: 10.3358/SHOKUEISHI.40.4_309
M. Horie, R. Ishii, Terumitsu Yoshida, Youji Hoshino, H. Nakazawa
A simple and rapid method using liquid chromatography-electrospray ionization-mass spectrometry (LC/MS-ESI) has been developed for the determination of macrolide antibiotics, erythromycin and oleandomycin, in meat and fish. The LC separation was carried out on a TSK-gel ODS 80-Ts column (150×2mm) by using 0.1% acetic acid-acetonitrile (65:35) as the mobile phase at a flow rate of 0.2mL/min. The positive ionization produced typical (M+H)+ molecular ions of both drugs (erythromycin m/z 734; oleandomycin m/z 688). The calibration graphs for erythromycin and oleandomycin were rectilinear from 0.05 to 10ng with selected ion monitoring (SIM). The drugs were extracted with 0.1% metaphosphoric acid-methanol (5:5), and the extracts were cleaned up on an OASIS HLB cartridge (60mg). The recoveries of the drugs from meat and fish fortified at a level of 0.2μg/g were 79.4-95.4%, with high precision. The limits of quantification of both drugs in meat and fish were 0.01μg/g.
建立了液相色谱-电喷雾-质谱联用(LC/MS-ESI)快速测定肉类和鱼类中大环内酯类抗生素红霉素和夹竹桃霉素的方法。色谱柱为TSK-gel ODS 80-Ts (150×2mm),流动相为0.1%醋酸-乙腈(65:35),流速为0.2mL/min。正电离产生典型的(M+H)+分子离子(红霉素M /z 734;夹竹桃霉素m/ z688)。在选择离子监测(SIM)下,红霉素和夹竹桃霉素在0.05 ~ 10ng范围内呈直线关系。用0.1%偏磷酸-甲醇(5:5)提取药物,用OASIS HLB药筒(60mg)清洗。在0.2μg/g水平下,加样回收率为79.4 ~ 95.4%,精密度高。两种药物在肉类和鱼类中的定量限均为0.01μg/g。
{"title":"Determination of Erythromycin and Oleandomycin in Meat and Fish by LC/MS","authors":"M. Horie, R. Ishii, Terumitsu Yoshida, Youji Hoshino, H. Nakazawa","doi":"10.3358/SHOKUEISHI.40.4_309","DOIUrl":"https://doi.org/10.3358/SHOKUEISHI.40.4_309","url":null,"abstract":"A simple and rapid method using liquid chromatography-electrospray ionization-mass spectrometry (LC/MS-ESI) has been developed for the determination of macrolide antibiotics, erythromycin and oleandomycin, in meat and fish. The LC separation was carried out on a TSK-gel ODS 80-Ts column (150×2mm) by using 0.1% acetic acid-acetonitrile (65:35) as the mobile phase at a flow rate of 0.2mL/min. The positive ionization produced typical (M+H)+ molecular ions of both drugs (erythromycin m/z 734; oleandomycin m/z 688). The calibration graphs for erythromycin and oleandomycin were rectilinear from 0.05 to 10ng with selected ion monitoring (SIM). The drugs were extracted with 0.1% metaphosphoric acid-methanol (5:5), and the extracts were cleaned up on an OASIS HLB cartridge (60mg). The recoveries of the drugs from meat and fish fortified at a level of 0.2μg/g were 79.4-95.4%, with high precision. The limits of quantification of both drugs in meat and fish were 0.01μg/g.","PeriodicalId":17269,"journal":{"name":"Journal of The Food Hygienic Society of Japan (shokuhin Eiseigaku Zasshi)","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1999-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87538040","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 9
期刊
Journal of The Food Hygienic Society of Japan (shokuhin Eiseigaku Zasshi)
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