Determination of Ampicillin in Serum by Using Simple Ultrafiltration Technique and Liquid Chromatographic Analysis

1986 ◽  
Vol 69 (5) ◽  
pp. 757-759
Author(s):  
James E Hutchins ◽  
Krystyna Tyczkowska ◽  
Arthur L Aronson

Abstract A new liquid chromatographic method for determination of ampicillin in canine and equine serum has been developed. The serum sample (500 μL) is vortex-mixed with 20% ethanol (500 μL) and filtered using a 30 000 molecular weight cutoff microseparation tube to separate high molecular weight solutes following low-speed centrifugation. Ampicillin is then separated from other serum components by reverse phase ion-pair liquid chromatography (LC). The ultraviolet (UV) absorbance of the column effluent is monitored at 230 nm. Recoveries of ampicillin from canine serum spiked at concentrations of 10, 40, and 60 μg/mL were 93.1,100.9, and 87.8%, respectively, with coefficients of variation (CVs) of 2.91, 3.08, and 4.08%, respectively. Recoveries of ampicillin from equine serum spiked at the same concentrations were 91.6, 90.1, and 88.7%, respectively, with CVs of 3.03, 2.61, and 3.35%, respectively. The limit of detection for ampicillin by this method is less than 0.5 μg/mL serum.

1986 ◽  
Vol 69 (5) ◽  
pp. 760-762
Author(s):  
Krystyna Tyczkowska ◽  
Arthur L Aronson

Abstract A sensitive liquid chromatographic method has been developed for the simultaneous determination of oxytetracycline, minocycline, tetracycline, and doxycycline in serum. A serum sample is vortex-mixed with a solution of mobile phase for tetracyclines and 2% (v/v) phosphoric acid. The mixture is filtered using a 30 000 molecular weight cutoff microseparation tube which separates high-molecular-weight solutes following low-speed centrifugation. Tetracyclines are separated from other serum components by reverse phase liquid chromatography (LC) with buffered methanol mobile phase. Ultraviolet absorbance of the column effluent is monitored at 267 nm. Concentrations as low as 0.2 μg/mL of tetracyclines in serum are quantitatable, with recoveries from 76.2 to 102.6% and coefficients of variation from 2.69 to 5.36%. The method has been tested in bovine, porcine, equine, caprine, ovine, canine, feline, and avian (turkey) serum.


1988 ◽  
Vol 71 (4) ◽  
pp. 773-775
Author(s):  
Krystyna Tyczkowska ◽  
Arthur L Aronson

Abstract A sensitive liquid chromatographic method was developed for determining oxacillin, cloxacillin, and dicloxacillin (simultaneously), and penicillin G, amoxicillin, carbenicillin, and ticarcillin in canine and/ or equine serum. The method involves filtering diluted serum through a 30 000 molecular weight cut-off filter and separating penicillins from other serum components by ion-pair liquid chromatography using a reverse-phase column eluted with acetonitrile-water solutions. The ultraviolet absorbance of the column effluent was monitored at 230 nm. Recoveries of oxacillin, cloxacillin, dicloxacillin, and penicillin G (spiked at 2.5 μg/mL), amoxicillin (spiked at 5 μg/ mL), and carbenicillin and ticarcillin (spiked at 10 μg/mL) from canine and equine serums ranged from 78.3 to 104.4% with coefficients of variation ranging from 3.35 to 5.95%. The limit of detection for these penicillins was 0.02-0.05 μg/mL


2012 ◽  
Vol 9 (3) ◽  
pp. 1327-1331 ◽  
Author(s):  
A. Narendra ◽  
D. Deepika ◽  
M. Mathrusri Annapurna

A reverse phase LC method was developed for the determination of Brimonidine in eye drops. Chromatography was carried on an Inertsil ODS 3V column (C18) using a mixture of Octane 1- sulfonic acid sodium salt (0.02M) (pH 3.5 ± 0.05) and acetonitrile (64:36 v/v) as mobile phase at a flow rate of 1 mL/min with UV detection at 254 nm. The drug was eluted at 4.636 min. The detector response was linear in the concentration range of 0.4–72 μg/mL. The limit of detection and limit of quantification were found to be 0.0561 and 0.1848 μg/mL respectively. The proposed method was validated as per the ICH guidelines and can be applied for the routine analysis of Brimonidine in eye drops.


1979 ◽  
Vol 25 (7) ◽  
pp. 1293-1296 ◽  
Author(s):  
P M Kabra ◽  
L L Tsai ◽  
L J Marton

Abstract We describe a specific and precise method for measuring concentrations of cortisol in serum or plasma by liquid chromatography. Cortisol, together with an internal standard, equilenin, is extracted from 1 mL of serum or plasma and analyzed isocratically on a reversed-phase column with a mobile phase of acetonitrile/phosphate buffer (30/70, by vol.), at a flow rate of 2.0 mL/min. The eluted cortisol is detected by its absorption at 254 nm and quantitated by peak height measurements. Each analysis requires no longer than 15 min at the optimum column temperature of 50 degrees C. The lower limit of detection for cortisol is about 2 ng/sample for a standard solution; sensitivity is routinely 5 micrograms/L of serum. Analytical recoveries exceeded 95%, with good day-to-day precision (coefficients of variation between 4 and 7%). Of more than 50 drugs and steroids tested for possible interference, only the steroids cortisone, prednisone, and prednisolone may interfere with the analysis of cortisol.


1983 ◽  
Vol 66 (4) ◽  
pp. 864-866
Author(s):  
Eileen S Bargo ◽  
◽  
E Aranda ◽  
C Bonnin ◽  
S Hauser ◽  
...  

Abstract A reverse phase high pressure liquid chromatographic method for the determination of oxazepam in tablets and capsules was collaboratively studied by 9 laboratories. Collaborators were supplied with 6 samples that included synthetic and commercial formulations. Tablet and capsule composites are diluted with methanol and filtered. Oxazepam is determined at 254 nm by using a C18 column. Mean recoveries of oxazepam from synthetic tablet and capsule formulations were 97.2 and 99.0%, respectively. Mean coefficients of variation for tablets and capsules ranged from 1.85 to 2.86%. The method has been adopted official first action.


1988 ◽  
Vol 71 (6) ◽  
pp. 1156-1157 ◽  
Author(s):  
Lawrence Felice ◽  
El Hassane Abdennebi ◽  
Muhammed Ashraf

Abstract A liquid chromatographic method is described for the measurement of thiamphenicol in bovine plasma. The plasma (1 mL) is extracted with ethyl acetate. After the solvent is evaporated under a stream of nitrogen, the residue is reconstituted in methanol-water and analyzed by reverse-phase liquid chromatography with UV detection at 224 nm. The intra-day recoveries for bovine plasma spiked with 5 and 50 μg/mL of thiamphenicol were 102 and 101%, respectively, with coefficients of variation of 2.40 and 0.28%, respectively. The interday recoveries for the 5 and 50 μg/mL samples were 103 and 101%, respectively, with coefficients of variation of 3.40 and 0.94%, respectively. The sensitivity of the method allows quantitation to at least the 100 ng/mL level


1988 ◽  
Vol 71 (6) ◽  
pp. 1123-1130 ◽  
Author(s):  
Susan Ting

Abstract A simple and rapid reverse-phase liquid chromatographic method was developed for the qualitative and quantitative analysis of 13 cephalosporin compounds. A mixture of cefaclor, cefadroxil, cefamandole nafate, cefamandole sodium, cefazolin, cefoperazone, cefotaxime, cefoxitin, ceftizoxime, cephalothin, cephalexin, cephapirin, and cephradine was resolved into its components in raw material and dosage form samples by using a Clg column, a methanol-water-acetic acid (30 + 70 + 0.1) mobile phase, and a UV detector set at 254 nm. The proposed method is suited both for the determination of cephalosporins in a wide variety of commercial dosage forms and for the investigation of related compounds and other impurities in samples of 7 of the cephalosporins


1982 ◽  
Vol 65 (6) ◽  
pp. 1362-1365
Author(s):  
Kazuo Nakao ◽  
Keiichi Honda ◽  
Tohru Yoneya

Abstract A sensitive high pressure liquid chromatographic method was developed for the determination of allantoin in cosmetic preparations. The procedure consists of simple cleanup of samples, derivatization with p-nitrobenzaldehyde in N,N-dimethylformamide to an ultraviolet labeled derivative, and reverse phase chromatography on an octadecylsilylated silica column. Ultraviolet absorbance was measured at 270 nm. Recovery was greater than 97% for cosmetic samples, and the minimum limit of detection was 10 ng.


2007 ◽  
Vol 57 (2) ◽  
pp. 231-239 ◽  
Author(s):  
Mohamed Rizk ◽  
Fawzia Ibrahim ◽  
Mohamed Hefnawy ◽  
Jenny Nasr

Micellar liquid chromatographic analysis of benzyl alcohol and benzaldehyde in injectable formulationsAn accurate, sensitive and selective reversed-phase micellar liquid chromatographic method was developed for simultaneous determination of benzyl alcohol and benzaldehyde. This method was applied in different injectable formulations containing diclofenac, piroxicam, lincomycin and clindamycin. The method showed excellent linearity in the range of 10-100 μg mL-1and 1-20 μg mL-1with the limit of detection (S/N = 3) 0.25 μg mL-1(2.3 x 10-6mol L-1) and 0.12 μg mL-1(1.13 x 10-6mol L-1) for benzyl alcohol and benzaldehyde, respectively. The suggested method was successfully applied to the analysis of the studied drugs in bulk with average recoveries of 100.1 ± 1.0% for benzyl alcohol and 100.4 ± 1.6% for benzaldehyde, and to the determination of benzyl alcohol and benzaldehyde in injectable formulations with the respective average recoveries of 99.8 ± 0.3 and 100.0 ± 0.4%.


1986 ◽  
Vol 69 (3) ◽  
pp. 490-492
Author(s):  
Stephen C Slahck ◽  
◽  
L B Aaron ◽  
O O Bennett ◽  
R M Elliott ◽  
...  

Abstract A liquid chromatographic method for determination of oxythioquinox (Morestan®) in oxythioquinox technical and formulated products has been developed and collaboratively studied in 14 laboratories. Samples are dissolved in chloroform containing n-valerophenone as an internal standard, diluted with acetonitrile, and analyzed by reverse phase chromatography. Collaborators analyzed blind duplicate samples of oxythioquinox technical and 25 WP. Coefficients of variation were 1.06 and 1.72% for the technical and 25 WP samples, respectively. The method has been adopted official first action.


Sign in / Sign up

Export Citation Format

Share Document