Automated determination of drugs in serum by liquid chromatography with column-switching. I. Separation of antiepileptic drugs and metabolites.

1988 ◽  
Vol 34 (1) ◽  
pp. 141-144 ◽  
Author(s):  
K Matsumoto ◽  
H Kikuchi ◽  
S Kano ◽  
H Iri ◽  
H Takahashi ◽  
...  

Abstract This is a fully automated system for determining six common antiepileptic drugs and two principal metabolites of carbamazepine in serum. It is based on "high-performance" liquid chromatography (HPLC), with column switching. TSKprecolumn BSA-ODS and TSKgel ODS-120A (both from Toyo Soda) were used as the precolumn and analytical column, respectively. The former contains octadecylsilyl resins treated with bovine serum albumin (BSA), and does not adsorb macromolecules such as serum proteins but retains small lipophilic molecules such as antiepileptic drugs. Serum samples are directly injected onto the precolumn. After washing out the serum proteins from the precolumn with sodium phosphate buffer, we switch the column connections to introduce the retained substances onto the analytical column and elute with a step-gradient of acetonitrile/sodium phosphate buffer. The high analytical recovery (95-102%) and the reproducibilities (CV less than 5% within-run) indicate that this system is suitable for use in theraputic drug monitoring in clinical laboratories.

1990 ◽  
Vol 36 (8) ◽  
pp. 1530-1530

Abstract Vol 35 p 1263: Right column, last paragraph, should read "P >0.05." pp 1437-1439: Printed Figure 2 should be Figure 5, printed Figure 3 should be Figure 2, printed Figure 4 should be Figure 3, and printed Figure 5 should be Figure 4. The legends were correct as printed. p 1541: The effects of adding citrate were obscured in the Table in the right column. The correct presentation is as follows: See table in the PDF file p 1582: A corrected Figure 1, showing the complementary sequences (instead of the genomic sequences) used for primers 461 and 459, is printed below. See image in the PDF file p 1672: Under Subjects, the 157 NIDD subjects were 112 women and 45 men. Vol 36 p 26: The illustrations for Figures 3 and 4 should be interchanged. p 629: The top and bottom panels in the Figure should be interchanged. p 909: In the Liquid chromatography section, the 0.1 mol/L sodium phosphate buffer was adjusted to pH 6.5 with 5 mL of triethylamine. p 1159: Lines 4-6 of abstract 968 from Baxter Healthcare Corp., Dade Division, should read as follows: "... polyclonal α-hOG antibody-coated tube and detected using a monoclonal anti-β-hCG antibody labeled with 125I. The two-step protocol has a total assay time of 75 mim..."


1989 ◽  
Vol 35 (3) ◽  
pp. 453-456 ◽  
Author(s):  
K Matsumoto ◽  
S Kanba ◽  
H Kubo ◽  
G Yagi ◽  
H Iri ◽  
...  

Abstract We describe automated column-switching high-performance liquid chromatography for determining nine tricyclic and tetracyclic antidepressants (TCAs) and their metabolites in human serum. TSKgel ODS-80TM and TSKprecolumn PW (Tosoh Co., Tokyo) are used in the analytical column and the precolumn, respectively. A 200-microL serum sample is directly injected onto the precolumn. After washing the serum proteins from the precolumn with potassium phosphate buffer, the precolumn connection is switched to introduce the retained substances onto the analytical column. The drugs are then eluted within 30 min with an acetonitrile/potassium phosphate buffer mixture containing sodium 1-heptanesulfonate. The analytical recoveries (95-104%), reproducibilities (within-run CV less than 3%), and detection limits (10 micrograms/L) indicate that this HPLC system is suited for therapeutic drug monitoring. Correlations were good between the TCA concentrations in serum and administered dose (r = 0.713, n = 41), and between 10-hydroxynortriptyline and nortriptyline in serum (r = 0.691, n = 24).


2008 ◽  
Vol 93 (2) ◽  
pp. 569-574 ◽  
Author(s):  
L. Haifeng ◽  
L. Yuwen ◽  
C. Xiaomin ◽  
W. Zhiyong ◽  
W. Cunxin

2019 ◽  
Vol 86 (3) ◽  
pp. 374-376 ◽  
Author(s):  
Vitaly L. Spitsberg ◽  
Liza Ivanov ◽  
Vladimir Shritz

AbstractIn this Research Communication we present a study of the effect of Ca-binding salts on the recovery of milk fat globule membrane (MFGM) from buttermilk. Sodium phosphate buffer was used for the purpose of MFGM recovery from buttermilk for the first time and we showed that 0.1 M buffer at pH 7.2 was the most effective for the recovery of MFGM. The fact of high efficacy of sodium phosphate buffer in recovery of MFGM from buttermilk allowed us to suggest that MFGM in buttermilk is present in association with casein through Ca- bridges formed between phospholipids of MFGM and phosphate groups of casein, primarily with k-casein as the peripheral protein of casein micelles.


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