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Hydroxylamine in Root Nodules

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Hydroxylamine in Root Nodules HYDROXYLAMINE IN ROOT NODULES BY M. DAMODARAN AND KERALA VARMA (From the University Biochemical Laboratory, Madras) Received November 4, 1943 HYDROXYLAMINE was postulated as an intermcdiate in nitrogen metabolism in the plant long before there was any experimcntal cvidcnce to support the vicw. Maz6 (1920) for example suggestcd the hypothesis that in photosyn- thesis hydroxylamine (formed from nitratc and ammonia) reacted with car- bonic acid giving rise to glycolaldehyde and nitrous acid. The possibility of amino-acids being formed by reaction betwcen nitrogen-free organic compounds and hydroxylamine was suggcstcd by Baly and Stern (1923). Experimental cvidcnce for the cxistence of hydroxylamine in plants and in symbiotic bacteria has however been obtained only recently. Blom (1931) detected traces of hydroxylaminc in Azotobacter culturcs while Lcmoigne et al. (1935) and Endres (1935) were able to show that such cultures con- tained carboximcs which on hydrolysis yielded free hydroxylamine. Lcmoigne et al. (1937) claim to have found volatile compounds of hydroxylamine in the fresh leaves of higher plants. Virtanen et al. (1938) in their study on the excretion of nitrogenous material by root nodules isolated the oxime of oxalacctic acid as its copper salt. As aspartic acid was also found among the products of excretion, Virtanen suggcstcd that amino-acid synthesis by symbiotic bacteria takes place according to the following reactions : Ns-.->NH2OH-->COOH.C (NOH).CH2.COOH-~COOH-CH (NH2). CH2.COOH->othcr amino-acids (by transamination according to Braun- stein and Kritzman, 1937). Thcsc conclusions are of far-reaching impor- tance and require detailed substantiation. Since the fact of excretion of nitrogenous material by legume bacteria has itself been questioned (Wilson et aL, 1938; Bond, 1937), in the prescnt investigation, root nodules grow- ing on several spccies of leguminous plants have becn cxamincd for their content of frce and combined hydroxylamine. For the quantitative cstima- tion of hydroxylamine a highly spccific colorimetric method* has been work- ed out based upon its convcrsion to nickel dimcthylglyoxime. By conden- sation with diacetylmonoxime in the presence of a large excess of the latter * A note on the method was published in Current Science, 1943, 12, 79. 9 B~ 10 M. Damodaran and Kerala Varma and under suitable conditions of temperature and pH hydroxylamine is quantitatively converted into dimethylglyoxime which is readily estimated by the rose-red colour which it gives on treatment with oxidised nickel solution (Feigl, 1924). Hydroxylamine in concentrations of 0.0005 rag. nitrogen per ml. can be estimated by this procedure. For application to plant material a trichloracefic acid extract of the latter is prepared, hydrolysed to liberate combined hydroxylamine if the latter is also to be determined and after neutralization treated with diacetyl- monoxime. The dimethylglyoxime produced is extracted out with ether, the ether removed by evaporation, the residue taken up in alcohol and the dimethylglyoxime present estimated colorimetrically by means of nickel. Applying this proceedure to root nodule material, no free hydroxyl- amine was found in the nodules of any of the several species examined. If however root nodule extracts were first submitted to a prefiminary hydro- lysis by keeping at 100~ C. for 6 hours in 3N sulphuric acid, considerable quantities of hydroxylamine appeared. Similar results were obtained when combined hydroxylamine was determined by the method described by Blom (1926). These results are summarised in Table I. TABLE I Combined hydroxylamine in root modules mg. hydroxylamine-N per 100 g. nodules Present method Blom's method 1. Phaseolus mungo (Green gram) .. 7" 595 7" 789 2. Vigna cat]ang (Karamani) .. 7-084 7.075 3. Phaseolus radiatus (Black gram) .. 6" 745 6" 738 4. Dolichos biflorus (Horse gram) .. 4"751 4-746 5. Pithecolobium saman (Rain tree) .. 8-742 8- 737 6. Pongamia glabra (Pungu) .. .. 9-177 9" 165 Experimental Reagents.--(a) Hydroxylamine standard, containing 0-01 nag. hydroxy- lamine-N in 1 ml. 4.953 mg. hydroxylamine hydrochloride dissolved in 100 ml. The solution is stable for over two weeks. (b) Diacetylmonoxime in N/10 ammonia, 5.6 g. dissolved in 10 ml. of N ammonia and diluted with water to I00 ml. (c) Oxidised nickel solution 0.4479 g. nickel sulphate (NiSO4 6H~O) dissolved in 1 litre. For each estimation 10 ml. of the so!ution are treated Hydroxylamine in Root Nodules 11 with saturated bromine water added drop by drop till a distinct excess is present. After allowing to stand for 15 minutes normal ammonia is added drop by drop till excess bromine is decolorized. Procedure.--The test solution containing between 0.025 and 0,075 rag. hydroxylamine-N is neutralised to pH 7.2 by the addition of ammonia and then treated with 1 ml. of diacetylmonoxime solution (B). After allowing to stand for half-an-hour at room temperature, 10 ml. of the oxidised nickel solution (C) are added and mixed and after five minutes made up to 25 ml. The rose-red colour which develops is compared with a standard hydroxylamine solution (A), 5 ml. of which are subjected to the same treatment as the test solution. Proportionality between colour and concentration.--Comparison of the colour developed with hydroxylamine solutiovs of different concentratiors varying from 0.025 to 0.075 mg. N in 25 ml. showed that within this range there is reasonably good proportionality between colour and concentratiov., so that estimation can be made of a solution containing 0.001 mg. hydroxyl- amine-N per ml. with an error of less than 4~o, the accuracy being higher with concentrations more closely approaching that of the standard (Table II). Concentrations down to 0.0005 mg. hydroxylamine-N can be deter- mined using a standard of half the strength of the foregoing (Table III). TABLE II Standard : 0.05 rag. hydroxylamine-N Standard and test solution made up to 25 ml. Reading of standard : 20 mg. hydroxyl- Readings Readings % error amine-N in test calculated found (--) solulion 0"02 O" 025 46:o 4i:3 3:~5 0"03 33"3 34"3 3"0 O" 035 28-6 29.3 2"4 0"04 25"O 25.3 1"2 0"045 22"2 22.4 0"9 0"055 18-2 18-3 0"55 0"06 16"7 16"9 I-2 0"065 15"4 15"7 1"94 0"07 14-2 14-6 2-8 O" 075 13"3 13"7 3"0 12 M. Damodaran and Kerala Varma TABLE III Standard : 0.025 mg. hydroxylamine-N Standard and test solution made up to 25 rot. Reading of standard : 20 mg. hydroxyl- Readings Readings error amine-N in test calculated found solution 0.01 0.0125 46~o 4i'7 4:25 0.015 33-3 34-5 3.6 0-0175 28.6 29.4 2-~ 0.02 25.0 25.6 2"4 0.0225 22.2 22.5 1"39 0.0275 18.2 18.4 I'~ 0.03 16.7 17.0 1.2 0-0325 15.4 15.8 2"6 0.035 14.2 14.7 3"52 O" 0375 13.3 13"9 4"5 Effect of Temperature.--In the preparation of dimethylglyoxime the condensation between diacetylmonoxime and hydroxylamine has been car- ried out at various temperatures, e.g., at 100 ~ C. by Adams and Kamm (1918) and at 70 ~ C. by Semon and Damerell (1925). Consequently in the earlier experiments the reaction mixture containing the test solution and diaeetylmonoxime was placed in a boiling water-bath. It was found how- ever that the reaction was incomplete at this temperature. The effect of temperature of condensation on the colour values obtained are shown in Table IV which summarizes the results of experiments in which the colour TABLE IV Standard : 0.05 mg. hydroxylamine-N Condensation with diacetylmonoxime at room temperature for half-an-hour Test solution : condensation with diacetylmonoxime at different temperatures Standard and test solution made up to 25 ml. Reading of standard : 20 % Error at the various reaction temperatures mg. hydroxyl. At room At 75 ~ C. I At 75 ~ C. At 75 ~ C. At 100 ~ C. At 100 ~ C. amine-N in test temperature for [ for for for for solution for 88hour 88hour 89hour 1 hour 88hour 89hour 0.02 3.5 4.0 4.75 5"0 5.5 6-8 0.03 3.0 3"6 4"5 4"8 5.0 6.0 0.035 2-79 2-9 3-5 3-87 4"9 5"2 0.04 2.0 2.2 2.4 3-2 3.6 4"4 0.045 0-9 1.35 1"78 2.25 2.2 4"I 0-055 0-55 1-1 1-1 1.64 2"7 4"4 0-06 1-2 2.0 2"39 2.99 3.2 5"1 O. 065 1-94 2.9 3"2 3"8 4"5 5-8 0-07 3-2 3-5 3-5 4"2 4"9 6"3 O. 075 3.7 4.0 4"5 4"8 5"3 6"3 Hydroxflamine in Root Nodules 13 produced at different reaction temperatures was compared with that at room temperature taken as standard. Colour intensity is always lower at the higher reaction temperatures. Effect of Alkalinity.--In the usual preparation of dimethylglyoxime no special attention appears to have been paid to control the degree of alka- linity at which the reaction between diacetylmonoxime and hydroxylamine takes place. Using diacetylmonoxime dissolved in different concentrations of ammonia, it was found that the reaction proceeded best at pH 8.8 to 9 which was obtained by dissolvil~g the diacetylmonoxime in N/10 ammonia under the conditions described.
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