• Journal of the Korean Applied Science and Technology
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• v.33 no.3
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• pp.459-465
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• 2016

This study investigated reusability of costly guard column by ultrasonic. It also investigated various effects that affect to guard column generation by ultrasonic. When investigated 30 KHz of frequency, area of ascorbic acid is 73.0% compared to unused guard column. As a result of investigation of effect of pH, guard column by ultrasonic is effective at alkali area. As a result of investigation of solvent effect, when ethanol is used, generation rate is 81.9% as of peak area compared to the case of analysis in un used column. From the result, it indicates that regenerated guard by ultrasonic is reusable.

• Journal of environmental and Sanitary engineering
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• v.21 no.4 s.62
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• pp.29-38
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• 2006

This study included the development of analytical method for determining perchlorate in water sample. The analytical condition was referred in EPA 314.0 method which use ion chromatography and the concentrator column was replaced by the guard column. Concentrating 10mL raw or treated water sample on to AGl6 guard column made it possible to get the LOD(Limit of Detection) of $0.73\;{\mu}g/L$. The total run time was 11 minutes and during run time next sample could be concentrated on AGl6 guard column. Compared to the Concentration method which needed manual operation, the Direct Injection method could screen the many water samples. The LOD of the Direct Injection method was higher and the sensitivity was lower than that of the Concentration method. The RSDs(Relative Standard Deviations) were lower than 2.5 % for peak height and 0.7 % for retention time in pre-concentration methods. This method Showed good reproducibility and reliability and it was thought the deviations of recovery value could be reduced by considering column capacity and making water sample homogeneous. Matrix Elimination could be done using the pre-concentration method if perchlorate were in complex matrix of sample.

• FOCUS: LIFE SCIENCE
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• no.1
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• pp.5.1-5.3
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• 2024

The document discusses the regeneration of Partisil/Partisphere ion-exchange columns in chromatography. It mentions that column efficiency can diminish with use due to the accumulation of sample and/or mobile phase impurities at the head of the column. This can lead to a change in back pressure, lower column efficiency, and sometimes a change in selectivity. The document outlines a procedure that may restore column performance. The document also provides everyday practices to enhance the lifetime of a column. These include using only high-purity HPLC solvents and buffers, using freshly prepared mobile phases and buffers, filtering mobile phases to remove particulates, using appropriate sample clean-up procedures, using a guard column or pre-column filter, and working within the pressure and flow rate limitations of the column. For the regeneration of Partisil/Partisphere SAX, SCX, WAX, and WCX columns, the document suggests passing 20 column volumes of various mobile phases through the column. These include a buffer wash, distilled water, an acid wash, a chelating wash, a methanol wash, and a buffer for separation. The document emphasizes that not all of these wash steps are required for every column clean-up and that some chromatographers require only a combination of certain steps.

• FOCUS: LIFE SCIENCE
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• no.1
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• pp.1.1-1.4
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• 2024

This article provides comprehensive guidance on the maintenance, cleaning, regeneration, and storage of silica-based HPLC (High-Performance Liquid Chromatography) columns. The general considerations emphasize the importance of using in-line filters and guard cartridges to protect columns from blockage and irreversible sample adsorption. While these measures help, contamination by strongly adsorbed sample components can still occur over time, leading to an increase in back pressure, loss of efficiency, and other issues. To maximize column lifetime, especially with UHPLC (Ultra-High Performance Liquid Chromatography) columns, it is advisable to use ultra-pure solvents, freshly prepared aqueous mobile phases, and to filter all samples, standards, and mobile phases. Additionally, an in-line filter system and sample clean-up on dirty samples are recommended. However, in cases of irreversible compound adsorption or column voiding, regeneration may not be possible. The document also provides specific recommendations for column cleaning procedures, including the flushing procedures for various types of columns such as reversed phase, unbonded silica, bonded normal phase, anion exchange, cation exchange, and size exclusion columns for proteins. The flushing procedures involve using specific solvents in a series to clean and regenerate the columns. It is emphasized that the flow rate during flushing should not exceed the specified limit for the particular column, and the last solvent used should be compatible with the mobile phase. Furthermore, the article outlines the storage conditions for silica based HPLC columns, highlighting the impact of storage conditions on the column's lifetime. It is recommended to flush all buffers, salts, and ion-pairing reagents from the column before storage. The storage solvent should ideally match the one used in the initial column test chromatogram provided by the manufacturer, and column end plugs should be fitted to prevent solvent evaporation and drying out of the packing bed.

• Analytical Science and Technology
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• v.19 no.5
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• pp.383-388
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• 2006

Simple post-wash method by ion chromatography (IC) was established for the rapid and precise determination of fluoride ion in wastewater from mine in fluorite mineralized area. High sulfate in sample was retained in a pre-column and less strongly held fluoride ion was transferred to the principal separation system using modified conventional IC with switching technique. An analytical column with high capacity (AS 9 HC) was used as a pre-column to retain the amount of high sulfate. A guard column (AG 14) as a separation column was used to increase the response of fluoride and reduce the system pressure. According to the recovery of fluoride ion with one detector and the observation of sulfate peak with another conductivity detector, the optimum switching time of 10-port chromatographic injector was 4.3 min. The limit of detection (S/N = 3) of fluoride in synthetic solution containing $500mg\;L^{-1}$ sulfate was $2.4{\mu}g/L$, with $25{\mu}L$ sample volume.

• Journal of the Korean Society of Marine Environment & Safety
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• v.13 no.1 s.28
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• pp.61-67
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• 2007

This paper describes the implementation procedures and results of Fishery Safety and Security System to secure an aquaculture area from a thief. The system designed with various functional modules to implement selectively available system providing low cost to high cost and simple function to high function according to user's requirement in a practical fishing fields. In the abalone farm field located in Jin island, Jeonranam province and having condensed aquaculture facilities with 50 cages (10 row by 5 column) within 0.5 miles from coast, practical field tests are carried out. As results from that tests, it is found that the system can guard not only the whole area of cultivating farm field but also each cages with detail.

• The Korea Journal of Herbology
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• v.22 no.4
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• pp.261-270
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• 2007

Objective : The 5-HMF was not index material suitable to do the quality control of Rehmanniae Radix Preparata. In this study, We estimated the changes of oligosaccharide contents in Rehmanniae Radix Preparata using high-performance anion-exchange chromatography with pulsed amperometric detection(HPAEC-PAD). Methods : The analysis of oligosaccharide was conducted by HPAEC-PAD with Carbopac PA1, $250{\times}4mm$, 5um, and Carbopac PA1 guard column. Column temperature was kept at $30^{\circ}C$. Elution was carried out at 1000 ${\mu}l/min$ with 70mM NaOH and the injection volume was $10{\mu}l$. Each component was detected by PAD. Results : Nine constituents were found from merchandising Rehmanniae Radix Preparata(MR), while seven constituents were found in various processed Rehmanniae Radix Preparata. Not all constituents were defined but stachyose and raffinose were found in all cases. And The most common constituents of Rehmanniae radix was stachyose. In the course of processing, most of stachyose and raffinose were decreased. Stachyose was decreased slowly in the course of processing with rice wine(RR), amomi and rice wine(AR), and crataegi and rice wine(CR). However stachyose was decreased rapidly in the course of processing with fresh rehmannia juice(FR). The method with crataegi and rice wine(CR) showed the smallest decrease of stachyose. And processing method with crataegi and rice wine(CR) showed the most abundant amount for stachyose after the nineth processing. Conclusion : The changes of oligosaccharides in the course of processing were a very important direct barometers to do the quality control and set up a standard of Rehmanniae Radix Preparata.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.6 no.1
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• pp.28-37
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• 1996

Benzidine, an aromatic amine used primarily in the manufacture of azo dyes, is recognized as a urinary bladder carcinogen in humans. In rats, mice, and hamsters, chronic exposure to benzidine resulted in tumors of the liver. The present study was undertaken to suggest analyzing the metabolites of benzidine with the optimal condition, identify the metabolites of benzidine, and observe time variance of the metabolites in the isolated perfusated rat liver. N-acetylbenzidine was synthesized by acetylation of benzidine with acetic anhydride and separated by thin layer chromatography(TLC) and high performance liquid chromatography(HPLC). To analysis benzidine and the metabolites of benzidine, HPLC operating condition has been optimized by means of preliminary experiment. The mobile phase consisted of acetonitrile(37%) in phosphate buffer, flow rate maintained at 1.0 ml/min. Optimal detective conditions were electrochemicaldetector(ECD) at 0.75 V for benzidine and N-acetylbenzidine and ultravioletdetector(UVD) at 287 nm for N,N'-diacetylbenzidine. The separation system was composed of a guard column and a separation column(Polymer C18, $4.6{\times}250cm$) at a temparature of $40^{\circ}C$. The perfusion system was equilibrated for 30 minutes before addition of benzidine to the perfusate. Samples of the perfusate were collected at time intervals(0, 10, 20, 30, 60, 90, 120 min) during the 2 hour perfusion. Before analyzing samples by HPLC/ECD/UVD, samples had been treated with sep-pak. Samples of perfusate analyzed by HPLC/ECD/UVD and the metabolites of benzidine in the isolated perfused rat liver were N-acetylbenzidine and N,N'-diacetylbenzidine. Benzidine metabolized over 60% during the initial 30 minutes of perfusion, extensively by 1 hour, and was undetectable in the perfusate. N-acetylbenzidine increased by 30 minutes of perfusion, declined. N,N'-diacetylbenzidine increased the 0-90 minutes period, remained constant during the 90-120 minutes period.

• YAKHAK HOEJI
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• v.51 no.2
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• pp.96-102
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• 2007

Measurement of globotriaosylceramide (Gb3, ceramide trihexoside) in urine has clinical importance for monitoring after enzyme replacement therapy in Fabry disease patients. The disease is an X-linked lipid storage disorder that results from a deficiency of the enzyme ${\alpha}$-galactosidase A (${\alpha}$-Gal A). The lack of ${\alpha}$-Gal A causes an intracellular accumulation of glycosphingolipids, mainly Gb3. A simple, rapid, and highly sensitive analytical method for Gb3 in urine was developed without labor-extensive pre-treatment by electrospray ionization MS/MS (ESI-MS/MS). Only simple 5-fold dilution of urine is necessary for the extraction and isolation of Gb3 in urine. Gb3 in diluted urine was dissolved in dioxane containing C17:0 Gb3 as an internal standard. After centrifugation it was directly injected and analyzed through guard column by in combination with multiple reaction monitoring mode of ESI-MS/MS. Eight isoforms of Gb3 were completely resolved from urine matrix. C24:0 Gb3 occupied 50% of total Gb3 as a major component in urine. Linear relationship for Gb3 isoforms was found in the range of 0.005${\sim}$5.0 ${\mu}$g/ml. The limit of detection (S/N=5) was 0.005 ${\mu}$g/ml and limit of quantification was 0.05 ${\mu}$g/ml for C24:0 Gb3 with acceptable precision and accuracy. Correlation coefficient of calibration curves for 8 Gb3 isoforms ranged from 0.9598 to 0.9975. This method could be useful for rapid and sensitive 1st line Fabry disease screening, monitoring and/or diagnostic tool for Fabry disease.

• Journal of Genetic Medicine
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• v.4 no.1
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• pp.45-52
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• 2007

Purpose : A simple, rapid, and highly sensitive analytical method for Gb3 in plasma was developed without labor-ex tensive pre-treatment by electrospray ionization MS/ MS (ESI-MS/MS). Measurement of globotriaosy lceramide (Gb3, ceramide trihex oside) in plasma has clinical importance for monitoring after enzyme replacement therapy in Fabry disease patients. The disease is an X-linked lipid storage disorder that results from a deficiency of the enzyme ${\alpha}$-galactosidase A (${\alpha}$-Gal A). The lack of ${\alpha}$-Gal A causes an intracellular accumulation of glycosphingolipids, mainly Gb3. Methods : Only simple 50-fold dilution of plasma is necessary for the extraction and isolation of Gb3 in plasma. Gb3 in diluted plasma was dissolved in dioxane containing C17:0 Gb3 as an internal standard. After centrifugation it was directly injected and analyzed through guard column by in combination with multiple reaction monitoring mode of ESI-MS/MS. Results : Eight isoforms of Gb3 were completely resolved from plasma matrix. C16:0 Gb3 occupied 50% of total Gb3 as a major component in plasma. Linear relationship for Gb3 isoforms w as found in the range of 0.001-1.0 ${\mu}g$/mL. The limit of detection (S/N=3) was 0.001 ${\mu}g$/mL and limit of quantification was 0.01 ${\mu}g$/mL for C16:0 Gb3 with acceptable precision and accuracy. Correlation coefficient of calibration curves for 8 Gb3 isoforms ranged from 0.9678 to 0.9982. Conclusion : This quantitative method developed could be useful for rapid and sensitive 1st line Fabry disease screening, monitoring and/or diagnostic tool for Fabry disease.