Gas Chromatographic Determination of Nonvolatile Organic Acids in Sap of Sugar Maple (Acer saccharum Marsh.)

1984 ◽  
Vol 67 (6) ◽  
pp. 1125-1129
Author(s):  
Joseph N Mollica ◽  
Maria Franca Morselli

Abstract Qualitative analysis of organic acids has never been reported for sugar maple sap, but only for its products, "sugar sand" and maple syrup. A gas chromatographic (GC) method is described for the simultaneous determination of up to 13 nonvolatile organic acids in sugar maple sap. Sap is filtered through Celite, and acids are isolated via cation- and anion-exchange chromatography. Reaction of dried acids with BSA [N,O-bis(trimethylsilyl)acetamide] in the presence of pyridine and methoxyamine hydrochloride yields the more volatile TMS (trimethylsilyl) esters. Oxalic, succinic, fumaric, L-malic, tartaric, cis-aconitic, citric, and/or shikimic acids were found in maple sap at concentrations ranging from less than 50 ppb to more than 45 ppm, depending on the particular acid and the date of sap flow. Percent recoveries and coefficients of variation for the acids at the 500 ppm level were 46.0 (3.2), 92.0 (2.9), 73.0 (0.77), 94.0 (2.0), 95.0 (−), 72.0 (−), and 97.0 (0.38), respectively. Various amounts of nonvolatile organic acids are reported in the sap of one sugar maple tree throughout a sap season, and of 3 individual maples during an early sap flow. Quantitation limits were as low as 15 ppb for individual acids in the analysis of a 100 mL sap sample. Esters were separated on a mixed liquid phase column of 4% SE-52/2% SE-30 on Chromosorb W-HP. They were identified by relative retention time, using a dual flame ionization detector. Naphthalene was used as the internal standard. Concurrent identification of pyruvic, malonic, glutaric, α-ketoglutaric, cis-aconitic, and isocitric acids with those previously mentioned is also possible.

1983 ◽  
Vol 29 (7) ◽  
pp. 1404-1407 ◽  
Author(s):  
F A Muskiet ◽  
G Jansen ◽  
B G Wolthers ◽  
A Marinkovic-Ilsen ◽  
P C van Voorst Vader

Abstract We describe a rapid method for determining cholesterol sulfate in plasma and erythrocytes. After its single-step isolation by means of anion-exchange chromatography cholesterol sulfate is hydrolyzed, trimethylsilylated, and determined by gas chromatography with flame ionization detection. 5 beta-Cholestan-3 alpha-ol sulfate is used as internal standard. The method enables simultaneous determination of dehydroepiandrosterone sulfate in plasma. We applied it for the diagnosis of seven patients with recessive X-linked ichthyosis. Concentrations are given for plasma and erythrocytes from four unaffected relatives of patients with X-linked ichthyosis, a patient with placental sulfatase deficiency, two patients with other types of ichthyoses, and 20 controls. The method may also be of use for the rapid isolation of other organic sulfates from biological material, as illustrated by a comparison of gas chromatograms of urine from a normal pregnant woman and that from a patient with placental sulfatase deficiency.


1980 ◽  
Vol 26 (6) ◽  
pp. 781-781
Author(s):  
Brian W Renoe ◽  
Jay M McDonald ◽  
Jack H Ladenson

Abstract Vol. 25 p 1766: Second paragraph, line four, the reference numbers cited should be (5-11); numbers of all subsequent citations above 10 in text should be increased by one, to correspond with the list of references. p 1828: In Figure 2, the label on the ordinate is not clear. It reads “counts/10 s × 10−3.” p 1930: Under “Determination of Concentrations in Human Plasma,” the injection of dihydroergotamine should be 0.5 mL of a 1 g/L solution. p 1931: Nine to 12 determinations of binding in the absence of nonradioactive standard were also used to construct the standard curves. p 1932: In the paragraph preceding Results and in the caption to Figure 3, the amount of compound 2 is 0.5 mg, not 1 mg. p 2020: In the preparation of phosphate buffer, the second sentence should read: “Dissolve 2.84 g of sodium diphosphate in 100 mL of de-ionized water (solution 2).” p 2021: In the section on extraction of serum under Procedures, the 10 µL of internal standard and 200 µL of sample should be added to 200 µL of phosphate buffer. Vol. 26 p99: In the caption for Figure 3A, read “r = 0.99,” not “r = 0.09.” p. 176: The sample volume referred to in the fourth paragraph of column three should be 0.15 µL, not “150 mL.” p 193: Add to reference list: 8. Goutte-Coussieu, C., Habrioux, G., Eichenberger, D., and Jayle, M. F., Rapid fluorometry of estrogens in nonpregnancy urine, with use of chloroform extraction and purification by anion-exchange chromatography. Clin. Chem. 25, 230 (1979). 9. Jarrige, P., Purification et propriétés des sulfatases du suc d’Helix pomatia. Bull. Soc. Chim. Biol. (Paris) 7-8,761 (1963). 10. Ittrich, G., Untersuchungen über Extraktion des roten Kober-Farbstoffs durch organische Lösungsmittel zur Ostrogenbestimmung im Harn. Acta Endocrinol. (Copenhagen) 35, 34 (1960). 11. Adessi, G., Lallier, J. C., Goutte-Coussieu, C., and Jayle, M. F., Méthode de dosage automatique par spectrofluorimétrie des estrogénes urinaires au cours et en dehors de la grossesse. Ann. Biol. Clin. 37, 89 (1979). 12. Schöller, R., Contrôle de Qualité en Hormonologie. I.-Stéroides Urinaires. Editions Sepe, Paris-Fresnes, 1976, p 51. p. 354: In Table 1, last line, columns 2 and 4, substitute “0.12” for “0.16.”


1980 ◽  
Vol 26 (6) ◽  
pp. 781-781
Author(s):  
Brian W Renoe ◽  
Jay M McDonald ◽  
Jack H Ladenson

Abstract Vol. 25 p 1766: Second paragraph, line four, the reference numbers cited should be (5-11); numbers of all subsequent citations above 10 in text should be increased by one, to correspond with the list of references. p 1828: In Figure 2, the label on the ordinate is not clear. It reads “counts/10 s × 10−3.” p 1930: Under “Determination of Concentrations in Human Plasma,” the injection of dihydroergotamine should be 0.5 mL of a 1 g/L solution. p 1931: Nine to 12 determinations of binding in the absence of nonradioactive standard were also used to construct the standard curves. p 1932: In the paragraph preceding Results and in the caption to Figure 3, the amount of compound 2 is 0.5 mg, not 1 mg. p 2020: In the preparation of phosphate buffer, the second sentence should read: “Dissolve 2.84 g of sodium diphosphate in 100 mL of de-ionized water (solution 2).” p 2021: In the section on extraction of serum under Procedures, the 10 µL of internal standard and 200 µL of sample should be added to 200 µL of phosphate buffer. Vol. 26 p99: In the caption for Figure 3A, read “r = 0.99,” not “r = 0.09.” p. 176: The sample volume referred to in the fourth paragraph of column three should be 0.15 µL, not “150 mL.” p 193: Add to reference list: 8. Goutte-Coussieu, C., Habrioux, G., Eichenberger, D., and Jayle, M. F., Rapid fluorometry of estrogens in nonpregnancy urine, with use of chloroform extraction and purification by anion-exchange chromatography. Clin. Chem. 25, 230 (1979). 9. Jarrige, P., Purification et propriétés des sulfatases du suc d’Helix pomatia. Bull. Soc. Chim. Biol. (Paris) 7-8,761 (1963). 10. Ittrich, G., Untersuchungen über Extraktion des roten Kober-Farbstoffs durch organische Lösungsmittel zur Ostrogenbestimmung im Harn. Acta Endocrinol. (Copenhagen) 35, 34 (1960). 11. Adessi, G., Lallier, J. C., Goutte-Coussieu, C., and Jayle, M. F., Méthode de dosage automatique par spectrofluorimétrie des estrogénes urinaires au cours et en dehors de la grossesse. Ann. Biol. Clin. 37, 89 (1979). 12. Schöller, R., Contrôle de Qualité en Hormonologie. I.-Stéroides Urinaires. Editions Sepe, Paris-Fresnes, 1976, p 51. p. 354: In Table 1, last line, columns 2 and 4, substitute “0.12” for “0.16.”


2013 ◽  
pp. 767-769
Author(s):  
Maciej Wojtczak ◽  
Aneta Antczak-Chrobot ◽  
Krystyna Lisik

This study presents information about the usefulness of the high-performance anion exchange chromatography (HPAEC) method for the determination of some organic acids in beet white sugars and refined white cane sugars.


1976 ◽  
Vol 22 (6) ◽  
pp. 806-809 ◽  
Author(s):  
T R Keucher ◽  
E B Solow ◽  
J Metaxas ◽  
R L Campbell

Abstract We describe a modified method for assay of epsilon-aminocaproic acid. Serum or cerebrospinal fluid is deproteinized, followed by cation-exchange column-chromatography, and N-trifluoroacetyl-n-butyl derivatives of amino acids are formed and separated by gas chromatography. Tranexamic acid, a nonprotein amino acid, was used as an internal standard. The assay is sensitive and precise, and results correlate adequately with those obtained with an automated amino acid analyzer (ion-exchange chromatography).


1973 ◽  
Vol 19 (8) ◽  
pp. 817-820 ◽  
Author(s):  
S Katz ◽  
W W Pitt ◽  
G Jones

Abstract A simple, sensitive system has been developed for detecting oxidizable compounds that are eluted from chromatographic columns. It relies upon the production of fluorescent cerium(III) by the reaction of eluted compounds with cerium(IV) solution. When coupled with a modified ultraviolet-monitored anion-exchange chromatograph, this system provides excellent resolution and sensitivity in the analytical determination of aromatic organic acids.


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