Thin layer chromatographic separation and spectrodensitometric determination of higher and lower sulfonated subsidiary dyes in FD&C Yellow No. 6.

A thin layer chromatographic method is presented by which higher and lower sulfonated subsidiary dyes are simultaneously separated from FD&C Yellow No. 6. After separation, the colors are quantitated directly, using a spectrodensitometer. Recoveries of 1, 2, and 5% of added 1-(4-sulfophenylazo)-2-naphthol-3,6-disulfonic acid ranged from 92 to 111%. Recoveries of 1, 2, and 5% of added 1-(4-sulfophenylazo)-2-naphthol ranged from 90 to 110%.     

Prevention of hydrolytic rancidity in rice bran during storage.

The effect of microwave heating, packaging, and storage temperature on the production of free fatty acids (FFA) in rice bran was examined. Freshly milled raw rice bran was adjusted to 21% moisture content and heated in a microwave oven at 850 W for 3 min. Raw and microwave-heated rice bran were packed in zipper-top bags or vacuum-sealed bags and stored at 4-5 or 25 degrees C for 16 weeks. FFA content of bran was measured at 4-week intervals. Total FFA increased rapidly over the 16-week period from the initial value of 2.5% in raw bran stored at 25 degrees C to 54.9% in vacuum bags and 48.1% in zipper-top bags. However, total FFA of raw bran stored at 4-5 degrees C increased at a slower rate from an initial value of 2. 5 to 25.4% in vacuum bags and 19.5% in zipper-top bags. After 16 weeks of storage, total FFA of microwave-heated bran stored at 25 degrees C increased from 2.8 to 6.9 and 5.2%, respectively, for samples stored in vacuum bags and zipper-top bags. Total FFA of microwave-heated samples stored at 4-5 degrees C did not change significantly with storage time. Results showed that hydrolytic rancidity of rice bran can be prevented by microwave heating and that the recommended storage condition for microwaved rice bran is 4-5 degrees C in zipper-top bags.     

工厂化条件下氮处理对奶油生菜的生长及生理影响

通过水培试验研究不同氮处理(5 mmol·L~(-1)NO_3~--N、10 mmol·L~(-1)NO_3~--N和5 mmol·L~(-1)NO_3~--N+5 mmol·L~(-1)NH_4~+-N)对奶油生菜生长和生理特性的影响。研究结果表明,35 d后,总氮浓度相等时,NH_4~+-N抑制奶油生菜生长,该处理叶面积、株高、地上鲜重、地上干重、地下鲜重和地下干重分别降低78.2%、60.4%、87.0%、81.3%、80.1%和87.5%(P0.05),此外,两者的生理活性如根系活力、可溶性蛋白质、超氧化物歧化酶活性和硝酸还原酶活性均有显著性差异(P0.05)。与10 mmol·L~(-1)NO_3~--N(12.89 g)相比,5mmol·L~(-1)NO_3~--N(8.90 g)处理奶油生菜生物量稍微有所降低,叶面积、根长和地下干重分别降低48.1%、50.3%和37.5%(P0.05),而叶可溶性糖含量和花青素相对含量分别升高67.5%和51.9%(P0.05),而对NO_3~--N的吸收两者的比值在第21 d达到最大值,后者是前者的3.15倍。研究结果表明奶油生菜是喜硝蔬菜,且生菜的硝态氮适宜浓度前期(前21 d)为高浓度(10 mmol·L~(-1)),以便促进奶油生菜生长,后期(21 d后)可改为低浓度(5 mmol·L~(-1))以提高品质。     

Comparison of high pressure liquid chromatographic and chemical methods for vitamin D3 concentrates. II. Collaborative study.

A collaborative study was carried out which compared the official chemical method, 43.B14-43.B24, the official rat bioassay, 43.165, and the high pressure liquid chromatographic method for vitamin D3 resin, vitamin D3 resin in oil, and dry concentrate. A total of 340 samples were distributed to 17 collaborators for analysis. Five laboratories performed both the chemical and HPLC methods on 5 sets of blind duplicates. A 2-way analysis of variance comparing both methods for each sample showed a significant (P less than 0.01) difference between methods only for Sample 5. When the 2 methods were compared over all the samples, no significant (P less than 0.05) difference was found. Except for Sample 5, there were no differences in the repeatability of the methods. Per cent recoveries on Sample 3, which contained exactly 0.200 X 10(6) IU/g, showed 98.2% for the chemical method and 100.6% for the HPLC method for the 5 laboratories that performed both methods. The assay results of the HPLC and chemical methods are in good agreement with those found by the biological assay on Samples 1-4, but not for Sample 5. Evidence indicates that Sample 5 degraded partially to isotachysterol, and while the HPLC method yielded a reasonable value on this material, the chemical method erroneously showed full potency. An amendment is included for the collaboratively studied HPLC method which detects and eliminates 5,6-trans-vitamin D3, a possible interferant.     

灌溉条件下施氮水平对土壤 作物系统中肥料氮素去向的影响

本试验利用１５Ｎ示踪技术，研究３种施氮水平（适宜施氮量Ｎ１０∶１５０ｋｇＮ·ｈａ－１，低于适宜施氮量的５０％Ｎ０５∶７５ｋｇＮ·ｈａ－１，高于适宜施氮量的５０％Ｎ１５∶２２５ｋｇＮ·ｈａ－１）对灌溉冬小麦氮素利用、去向及作物产量的影响。结果表明：在灌溉条件下，３种施氮水平（Ｎ０５，Ｎ１０，Ｎ１５）的冬小麦氮素利用效率分别为３８５％、３２３％和２２４％，以Ｎ０５水平为最高。Ｎ１０施氮水平获得了最高的作物产量（６８０×１０３ｋｇ籽粒·ｈａ－１，１４７×１０３ｋｇ生物量·ｈａ－１），Ｎ０５水平同Ｎ１０水平相比，在产量上没有显著性差异；而Ｎ１５水平因施氮过量造成籽粒产量明显下降，与不施肥相比，差异不显著。在深层条施（５～８ｍｍ）条件下，仍有３０２％～３６７％的化学氮素通过各种途径而损失。在Ｎ１５水平中，施用氮素的４６％仍存在于０～５０ｃｍ土层中，远远高于其它两种施肥水平。土壤残留态的无机氮素含量以Ｎ１５施氮水平为最高     

Methodology for recognition of invasive potential of Escherichia coli.

Surveillance for dysentery-related invasive potential in bacteria using the Sereny keratoconjunctivitis test is restricted by expense, time factor, and necessity for confirmation. Primary screening of isolates in a standardized mammalian cell culture system is recommended. Bacteria are grown 20 hr in veal infusion, washed, and resuspended in 20% heat-inactivated fetal bovine serum (FBS) supplemented with 0.12% brain heart infusion and 0.1% bile salts. The HeLa culture is grown 20 hr as a monolayer in chamber slides with 90% minimal essential medium (MEM)-10% FBS. The host culture is infected at a ratio of 10 bacteria/mammalian cell for 3 hr at 35 degrees C. The infection medium is replaced with MEM-FBS supplemented with 300 microng lysozyme and 5 microng gentamycin/ml. The infected monolayer is incubated 5 hr at 35 degrees C to permit intracellular multiplication. Specimens are washed, fixed with methanol, and stained successively with May-Grunwald and Giemsa dyes. Bacteria occur within the cytoplasm if invasion has occurred. The criterion for a positive test is that 1% of the host cells possesses at least 5 bacteria in 2 of 3 trials. Invasiveness is correlated with and possibly preconditioned by cytotoxic principle(s). Infectivity rates vary from 0 to 30%. The cytopathic effect is noted in 5-50% of HeLa cells. Positive results must be confirmed by the Sereny test.     

Physicochemical and structural characterization of alkali soluble lignins from oil palm trunk and empty fruit-bunch fibers.

Six alkali soluble lignin fractions were extracted from the cell wall materials of oil palm trunk and empty fruit-bunch (EFB) fibers with 5% NaOH, 10% NaOH, and 24% KOH/2% H(3)BO(3). All of the lignin fractions contained rather low amounts of associated neutral sugars (0.8-1.2%) and uronic acids (1.1-2.0%). The lignin fractions isolated with 5% NaOH from the lignified palm trunk and EFB fibers gave a relatively higher degree of polymerization as shown by weight-average molecular weights ranging between 2620 and 2840, whereas the lignin fractions isolated with 10% NaOH and 24% KOH/2% H(3)BO(3) from the partially delignified palm trunk and EFB fibers showed a relatively lower degree of polymerization, as shown by weight-average molecular weights ranging between 1750 and 1980. The results obtained by alkaline nitrobenzene oxidation showed that all of the lignin preparations contained a high proportion of noncondensed syringyl units with small amounts of noncondensed guaiacyl and fewer p-hydroxyphenyl units. The lignin fraction extracted with 5% NaOH from the lignified EFB fiber was mainly composed of beta-O-4 ether-linked units. Small amounts of 5-5', beta-5, and beta-beta' carbon-carbon linkages were also found to be present between the lignin structural units. Further studies showed that uronic, p-hydroxybenzoic, and ferulic acids in the cell walls of palm fibers were esterified to lignin.     

Multiresidue screen for organophosphorus insecticides using gel permeation chromatography--silica gel cleanup.

A multiresidue screen for quantitative determination of 43 organophosphorus insecticides in 5 g of plant and animal tissues is described. The organophosphorus insecticides are extracted with methanol-dichloromethane (10 + 90, v/v) and cleaned up using automated gel permeation chromatography with hexane-ethyl acetate (60 + 40) eluant and in-line silica gel minicolumns. Concentrated extracts are analyzed by gas chromatography with flame photometric detection. The method recovers 43 organophosphorus insecticides in the range of 72 to 115%. Analysis of fortified bovine liver (n = 5) shows an average 95.9 +/- 4.8% recovery at the 0.05 micrograms/g level and 93 +/- 3.8% at the 0.5 micrograms/g level. Analysis of fortified bovine rumen content (n = 5) shows an average 98 +/- 4.2% recovery at the 0.1 micrograms/g level and 98.7 +/- 2.8% at the 1 micrograms/g level. Method detection limits ranged from 0.01 to 0.05 micrograms/g for the compounds studied using a nominal 5 gram sample.     

Antifungal constituents of the essential oil fraction of Artemisia dracunculus L. Var. dracunculus

The isolation and structure elucidation of antifungal constituents of the steam-distilled essential oil fraction of Artemisia dracunculus are described. Antifungal activities of 5-phenyl-1,3-pentadiyne and capillarin against Colletrotichum fragariae, Colletrotichum gloeosporioides, and Colletrotichum acutatum are reported for the first time. The relative abundance of 5-phenyl-1,3-pentadiyne is about 11% of the steam-distilled oil, as determined by GC-MS. Methyleugenol was also isolated and identified as an antifungal constituent of the oil.     

一株耐碳酸盐Bacillus属细菌的鉴定与特性分析

本研究从松嫩平原pH值在10.0以上、植物难以生存的斑块状裸地中分离到一株细菌SA-5,经鉴定该菌株为革兰氏染色阴性,杆状,接触酶阳性,氧化酶阴性,菌落呈橙黄色的好氧细菌,可水解淀粉。抗逆特性分析显示,菌株SA-5可在高达275mmol/L Na2CO3或pH 12.0以及2.0mol/L NaCl培养基中生长,中性条件下生长明显受到抑制,其中对碳酸盐的耐受性远高于普通植物。根据16SrDNA序列等分析结果显示,菌株SA-5属于Bacillus属,仅与菌株Bacillus aurantiacus K1-5T相似性最高,为99%,与其余已发表菌株均低于97%。由以上结果可见,菌株SA-5是Bacillus属中一株嗜碱耐盐菌,并且菌株SA-5对耐碳酸盐基因的开发具有潜在的价值。     

Aerobic metabolism of diclosulam on U.S. and South American soils

Degradation of the sulfonanilide herbicide diclosulam was studied on nine soils from three countries to determine the rates and products of aerobic metabolism. Diclosulam was applied to four agricultural soils from the United States, three from Argentina, and two from Brazil at a rate of 0.1 ppm, equivalent to approximately twice the maximum field application rate of 52 g of active ingredient/ha. U.S. and Brazilian soils were incubated in the dark at 25 degrees C at 75% 0.3 bar moisture; Argentinean soils were incubated in the dark at 20 degrees C and 45% moisture holding capacity. Samples were analyzed up to one year after treatment. Two-compartment DT(50) and DT(90) values averaged 28 +/- 12 and 190 +/- 91 days, respectively. Three soil metabolites reached levels of >10% of applied in at least one soil and were identified as the 5-hydroxy analogue of diclosulam (5-OH-diclosulam), aminosulfonyl triazolopyrimidine (ASTP), and the 8-chloro-5-hydroxy analogue of diclosulam (8-Cl-diclosulam). The terminal products of diclosulam soil metabolism were mineralization to CO(2) and bound soil residues. Apparent sorption coefficients (K(d)) were determined on a subset of samples by extraction with a 0. 01 M CaCl(2) solution followed by an acidified acetone extraction. Initial sorption coefficients were similar to those obtained in a batch equilibrium study and averaged 1.1 L/kg for the six soils tested. K(d) coefficients for the metabolites, when available, tended to be slightly lower than that for diclosulam. Sorptivity of diclosulam and degradates increased with time.     

Aroma chemicals isolated and identified from leaves of Aloe arborescens Mill. Var. Natalensis Berger.

Extracts from leaves of aloe (Aloe arborescens Mill. var. natalensis Berger) were obtained using two methods: steam distillation under reduced pressure followed by dichloromethane extraction (DRP) and simultaneous purging and extraction (SPE). A total of 123 aroma chemicals were identified in the extracts obtained by both methods using gas chromatography and gas chromatography/mass spectrometry. There were 42 alcohols, 23 terpenoids, 21 aldehydes, 9 esters, 8 ketones, 6 acids, 5 phenols, and 9 miscellaneous compounds. The major aroma constituents of this extract by DRP were (Z)-3-hexenol (29.89%), (Z)-3-hexenal (18.86%), (E)-hexenal (7.31%), 4-methyl-3-pentenol (5.66%), and butanol (4.29%). The major aroma constituents of this extract by SPE were (E)-2-hexenal (45.46%), (Z)-3-hexenal (32.12%), hexanal (9.14%), (Z)-3-hexenol (1.60%), and 3-pentanone (1.41%). Terpenoids were also found as one of the major constituents. The fresh green note of aloe leaves is due to the presence of these C(6) alcohols and aldehydes as well as terpenoids.     

Determination of chlorinated pesticide residues in foods. I. Rapid screening method for chlorinated pesticides in milk.

A rapid analytical method for determining chlorinated pesticide residues in milk was developed. Thirteen pesticides were almost completely extracted. Ten mL samples of fortified milk were extracted 3 times with 20 mL portions of n-hexane as follows: (A) in the absence of water-soluble solvent; in the presence of (B) 1 mL acetonitrile; (C) 3 mL acetonitrile; (D) 5 mL acetonitrile; (E) 5 mL ethanol; (F) 5 mL acetonitrile and 1 mL ethanol. System F produced the highest pesticide recoveries but the lowest fat extraction, thus eliminating the necessity for liquid-liquid partitioning and minimizing Florisil column cleanup. Pesticide recoveries throughout the procedure were 94--103%. It was noticed, however, that the fat in high fat-containing raw milk is more readily extracted than that in commercial milk.     

Gas-liquid chromatographic determination of morphine, heroin, and cocaine.

Morphine, heroin, and cocaine are quantitatively determined with the same gas-liquid chromatographic system. The compounds are separated on a 6 ft X 2 mm id glass column packed with a 1:1 mixture of 5% SE-30 on 80--100 mesh Chromosorb W and 3% OV-17 on 80--100 mesh Varaport 30. The column is temperature-programmed. Flame ionization detector responses are measured with a computer-based data system. Heroin and cocaine are chromatographed directly; morphine is derivatized first. The procedure was evaluated with previously analyzed commercial and forensic samples. Accuracy and precision were 5 and 3%, respectively.     

溶磷复合菌剂筛选及其对山核桃幼苗的生物学效应

为探究不同溶磷复合菌剂对山核桃幼苗生物学效应的影响,本研究从山核桃根际土壤中分离获得3株溶磷菌:果胶杆菌Pectobacterium cypripedii(R7)、伯克霍尔德氏菌Burkholderia sp.(R8)、肠杆菌Enterobacter sp.(R9)和4株自生固氮菌株:解聚糖类芽孢杆菌Paenibacillus glycanilyticus(G2)、葡萄球菌Staphylococcus sp.(G3)、假单胞菌Pseudomonas sp.(G4)、芽孢杆菌Bacillus sp.(G5),分别组合筛选出4种复合菌剂(R7G5、R8G4、R8G5、R9G4),并以蒸馏水为对照(CK),将其接种于山核桃幼苗的土壤中,通过测定接种处理后幼苗各项生长和生理指标,评价复合菌株对山核桃幼苗的作用效果。结果显示,R9G4和R8G5复合菌剂在蒙金娜无磷培养基(PVK)连续培养5 d后溶磷量显著高于其他组合。所有复合菌剂对山核桃幼苗均有促生作用;其中R8G5复合菌剂比其他复合菌的总体促生效果更为明显,施用后山核桃幼苗的根长、根面积、总生物量、全磷含量和可溶性糖含量较CK分别增加了105.53%、89.07%、52.94%、55.23%和91.99%;而施用R9G4复合菌剂后山核桃幼苗净光合速率(Pn)和全磷含量的提升效果最佳,较CK分别增加了79.47%和58.16%。本研究结果为进一步研制山核桃苗期促生菌剂提供了理论依据。     

添加螯合剂诱导－栽培红叶菾菜（Beta vulgaris var. cicla L.）修复铅和镉污染土壤效果的研究

以雄安新区安新县重金属污染农田土壤为供试土壤,以Cd超积累植物红叶菾菜（Beta vulgaris var. cicla L.）为供试植物,设置不同浓度EDTA和柠檬酸（0,2.5,5,7.5,10 mmol kg?1）处理进行盆栽试验,探究螯合诱导－红叶菾菜修复Cd、Pb污染土壤的可行性。结果表明:（1）与对照相比,添加EDTA螯合剂使红叶菾菜生长及生物量均受到抑制,一定浓度柠檬酸处理能显著促进植物生长,5 mmol kg?1柠檬酸处理对植物株高、茎粗及生物量与对照相比的上升比例分别为4.52%、44.07%和50%;（2）添加EDTA螯合剂后土壤中Cd、Pb有效态含量相比对照分别提高了108.61% ~ 235.39%、67.98% ~ 224.16%,柠檬酸处理后土壤Cd、Pb有效态含量最大提高了180.07%、186.01%,EDTA对土壤重金属的活化效率显著高于柠檬酸;（3）通过对红叶菾菜地上部Cd、Pb含量及富集系数比较发现,EDTA更能促进红叶菾菜对Pb的吸收,柠檬酸更能促进红叶菾菜对Cd的吸收;（4）螯合剂处理后土壤中铵态氮、有效磷、速效钾含量显著增加。就本文试验条件、供试材料而言,螯合诱导－红叶菾菜修复铅镉复合污染土壤是可行的。     

High pressure liquid chromatographic determination of 4,4'-(diazoamino)-dibenzenesulfonic acid in FD&C yellow no. 6.

Fourteen analysts from 9 laboratories evaluated a high pressure liquid chromatographic procedure for the determination of 4,4'-(diazoamino)-dibenzenesulfonic acid (DAADBSA) in FD&C Yellow No. 6. Each collaborator analyzed 5 samples nominally containing 0-0.050% DAADBSA. The repeatability and reproducibility of the method are estimated to be 0.003% and 0.020%, respectively. The method has been adopted as offical fist action.     

High pressure liquid chromatographic determination of the five major alkaloids in Papaver somniferum L. and thebaine in Papaver bracteatum Lindl. capsular tissue.

A high pressure liquid chromatographic isocratic procedure is described for determining and quantitating the 5 major alkaloids narcotine, papaverine, thebaine, codeine, and morphine in Papaver somniferum L. and thebaine in Papaver bracteatum Lindl. Other papaveraceous alkaloids, including salutaridine, oripavine, laudanosine, isothebaine, cryptopine, alpinigenine, narceine, protopine, and gnoscopine, were also quantitated. The values for morphine, codeine, and thebaine in P. somniferum were in agreement within 5--9% with values obtained by the United Nations Narcotics Laboratory by other methods. In contrast to previously reported procedures, the advantage of this method is that no precolumn or other purification other than solvent extraction of the capsular tissue is necessary. Isocratic chromatography alone on a single column resolved the 5 major alkaloids.     

Reduction of Carpophilus freemani dobson (Coleoptera: nitidulidae) aggregation pheromone response by synthetic analogues.

Analogues of (2E,4E,6E)-5-ethyl-3-methyl-2,4,6-nonatriene, the major component of the aggregation pheromone of Carpophilus freemani Dobson (Coleoptera: Nitidulidae), were synthesized and the potency of these compounds in suppressing the response of C. freemani to its pheromone in a wind tunnel bioassay was determined. The most potent compounds reduced behavioral response to pheromone 83-96% when the inhibitors were present in 10-fold excess. These compounds are (1Z, 3E,5E)-1-methoxy-3-ethyl-5-methyl-1,3,5-heptatriene, (1E,3E, 5E)-1-cyclopropyl-3-ethyl-5-methyl-1,3,5-heptatriene, and (1Z,3E, 5E)-1-cyclopropyl-3-ethyl-5-methyl-1,3,5-heptatriene. In the presence of fermenting bread dough (a pheromone synergist), the most potent inhibitory compound, (1Z,3E, 5E)-1-cyclopropyl-3-ethyl-5-methyl-1,3,5-heptatriene, was less effective in reducing mean landings (69% vs 99%) than when dough was absent. This inhibitory compound causes a reduction of response to pheromone but does not cause a reduction of response to fermenting food-type volatiles such as fermenting bread dough. Analogues of pheromones that strongly reduce response to pheromones by insects might be useful as biochemical probes to study the pharmacophoric (three-dimensional structure) requirements for pheromone perception.     

草地早熟禾原生质体培养与融合

以草地早熟禾品种RugbyⅡ成熟种子诱导的松软胚性愈伤组织为材料,以酶解法分离出原生质体,进行了原生质体培养;利用PEG融合法对MidnightⅡ和Nuglade的原生质体进行了融合,获得了体细胞杂种愈伤组织。研究了不同酶液组成、酶解时间、愈伤组织继代时间和渗透压对草地早熟禾原生质体游离及生长的影响;预处理对亲本原生质体活力的影响和适宜的融合条件。结果表明:采用继代培养8～10d的胚性愈伤组织,在1.0%纤维素酶+1.0%离析酶+0.5%果胶酶+0.3%崩溃酶条件下,酶解14～17h可得到产量和活力较高的原生质体;原生质体在KM8P培养基中培养3d后出现第1次细胞分裂,2～3周后形成小细胞团,此时添换低渗培养基2～3次,有利于小细胞团持续分裂并形成愈伤组织;试验获得了草地早熟禾品种RugbyⅡ原生质体来源的愈伤组织;5mmol/ml碘乙酰胺处理Nuglade原生质体10min及40μg/ml罗丹明处理MidnightⅡ原生质体5min,能有效地使Nuglade和MidnightⅡ原生质体失活;两品种融合PEG(6000)适宜浓度35%,融合率为9.8%。