Effect of Mobile Phase on Loading Mass for Preparative Separation of Sanguinarine and Chelerythrine on a Reverse Phase Column

2004 ◽  
Vol 27 (10) ◽  
pp. 1491-1505 ◽  
Author(s):  
Fei Zhang ◽  
Bo Chen ◽  
Xu‐Biao Luo ◽  
Xiao‐Lan Zhu ◽  
Shou‐Zhuo Yao
1990 ◽  
Vol 73 (6) ◽  
pp. 893-895 ◽  
Author(s):  
Ajay G Patel ◽  
Ramanbhai B Patel ◽  
Mukeshbhai R Patel

Abstract A liquid chromatographic (LC) method has been developed for determination of clobetasone-17-butyrate In ointment using clobetasone propionate as an internal standard. Separation was carried out on a C18 reverse-phase column using water-methanol as a mobile phase. Methylparaben and propylparaben (both sodium salt) used as preservatives did not Interfere with separation. Compounds are detected photometrically at 235 nm. Mean assay results for 0.05% commercial ointments were 100.36% (n = 5). Mean recovery of clobetasone-17-butyrate added to commercial ointment was 99.89%.


1982 ◽  
Vol 65 (4) ◽  
pp. 791-797
Author(s):  
Juan F Muniz ◽  
C Timothy Wehr ◽  
H Michael Wehr

Abstract A single column reverse phase high pressure liquid chromatographic method is described for the determination of vitamins D2 and D3 in fluid milk. Resolution of vitamin D2 from D3 is helpful for use as an internal standard. The method involves overnight saponification at room temperature, extraction of unsaponifiables, precipitation of cholesterol, and aluminum oxide column cleanup. Sample extracts were chromatographed under isocratic conditions on a 10 μVydac reverse phase column using acetonitrile- methanol (90 + 10) as the mobile phase. In addition, a MicroPak MCH-5 reverse phase column with acetonitrile as the mobile phase was used with an automatic system for one product type. Thirty samples each of homogenized (3.8% fat), low fat (2.07c fat), and skim (≤0.5% fat) milk spiked with 200,400, and 600 IU vitamin D/qt were analyzed. Coefficient of variation (CV) and percent recovery for each product type and each spike level of vitamins D2 and D3 were calculated from 10 replicate analyses. Vitamin D2 recoveries for all product types at the 3 fortification levels varied from 85.2 to 99.7%; vitamin D3 recoveries varied from 85.9 to 98.8%. The minimum detectable quantity of vitamin D in milk was 15IU/qt.


1982 ◽  
Vol 30 (6) ◽  
pp. 2287-2290 ◽  
Author(s):  
Hisanobu Yoshida ◽  
Ikue Morita ◽  
Tsutomu Masujima ◽  
Hideo Imai

1984 ◽  
Vol 67 (6) ◽  
pp. 1058-1061
Author(s):  
Harvey L Kramer

Abstract A liquid chromatographic (LC) method is described for the determination of sodium fluoroacetate in meat baits and formulations. Baits were extracted with water, ultrafiltered, partitioned into butanone, back-partitioned into dilute base, and diluted with acetonitrile. Aqueous formulations of 1080 were diluted with acetonitrile. The solutions were esterified with p-bromophenacyl bromide, using crown ether catalysis, and chromatographed on a 10 μm reverse phase column. Ultraviolet absorbance was monitored at 260 nm. Samples spiked to contain 1 mg and 10 mg 1080/100 g meat gave recoveries of 84.0-103.4%.


1987 ◽  
Vol 70 (3) ◽  
pp. 538-540
Author(s):  
Ugo R Cieri

Abstract A method is presented for the liquid chromatographic (LC) determination of ergotamine tartrate in tablets that is applicable even in the presence of other ingredients such as phenobarbital, belladonna alkaloids, and caffeine. The sample is transferred to a volumetric flask, a small volume of formic acid is added to dissolve and stabilize the ergotamine, and the solution is diluted to volume with methanol. The solution is mixed and filtered through paper. The LC system consists of a Rheodyne injector fitted with a 20 μL loop and a C,18 reverse phase column; the mobile phase is acetonitrile-water-triethylamine (700 + 300 + 0.5). Ergotamine tartrate is determined fluorometrically at an excitation wavelength of 250 nm and an emission wavelength of 430 nm. Recovery studies were conducted at the 0.3 and 1.0 mg levels. Average recoveries were 99.6 and 100.8%, respectively; relative standard deviations (RSDs) were 1.08 and 2.21%, respectively. Some commercial preparations containing ergotamine tartrate in combination with other ingredients were also analyzed. The RSDs for 5 determinations of each of 2 ground composites were 0.09 and 0.34%.


2011 ◽  
Vol 99 (6) ◽  
pp. 325-334 ◽  
Author(s):  
P. Deepika ◽  
N. Sivaraman ◽  
K. N. Sabharwal ◽  
T. G. Srinivasan ◽  
P. R. Vasudeva Rao

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