scholarly journals Determination of Ephedrine Alkaloids in Human Urine and Plasma by Liquid Chromatography/Tandem Mass Spectrometry: Collaborative Study

2003 ◽  
Vol 86 (4) ◽  
pp. 643-656 ◽  
Author(s):  
William A Trujillo ◽  
Wendy R Sorenson ◽  
D Gray ◽  
J Laurensen ◽  
G Luo ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Human Urine ◽  
Collaborative Study ◽  
Internal Standard ◽  
Tandem Mass ◽  
Accuracy And Precision ◽  
Liquid Chromatography Tandem Mass ◽  
Negative Controls ◽  
Different Levels

Abstract A collaborative study was conducted to evaluate the accuracy and precision of a method for ephedrine-type alkaloids (i.e., norephedrine, norpseudoephedrine, ephedrine, pseudoephedrine, methylephedrine, and methylpseudoephedrine) in human urine and plasma. The amount of ephedrine-type alkaloids present was determined using liquid chromatography (LC) with tandem mass selective detection. The test samples were diluted to reflect a concentration of 5.00–100 ng/mL for each alkaloid. An internal standard was added and the alkaloids were separated using a 5 μm phenyl LC column with an ammonium acetate, glacial acetic acid, acetonitrile, and water mobile phase. Eight blind duplicates of human urine and eight blind duplicates of human plasma were analyzed by 10 collaborators. In addition to negative controls, test portions of urine and plasma were fortified at 3 different levels with each of the 6 ephedrine-type alkaloids at approximately 1, 2, and 5 μg/mL for urine and 100, 200, and 500 ng/mL for plasma. On the basis of the accuracy and precision results for this collaborative study, it is recommended that this method be adopted Official First Action for the determination of 6 different ephedrine-type alkaloids in human urine and plasma.

scholarly journals Determination of Ephedrine Alkaloids in Dietary Supplements and Botanicals by Liquid Chromatography/Tandem Mass Spectrometry: Collaborative Study

2003 ◽  
Vol 86 (4) ◽  
pp. 657-668 ◽  
Author(s):  
William A Trujillo ◽  
Wendy R Sorenson ◽  
J Laurensen ◽  
G Luo ◽  
R McClanahan ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Dietary Supplements ◽  
Collaborative Study ◽  
Internal Standard ◽  
Negative Control ◽  
Interlaboratory Study ◽  
Tandem Mass ◽  
Accuracy And Precision ◽  
Ephedra Nevadensis

Abstract An interlaboratory study was conducted to evaluate the accuracy and precision of a method for ephedrine-type alkaloids [i.e., norephedrine (NE), norpseudoephedrine (NPE), ephedrine (E), pseudoephedrine (PE), methylephedrine (ME), and methylpseudoephedrine (MPE)] in dietary supplements and botanicals. The amount of ephedrine-type alkaloids present was determined using liquid chromatography with tandem mass selective detection. The samples were diluted to reflect a concentration of 0.0200 to 1.00 μg/mL for each alkaloid. An internal standard was added and the alkaloids were separated using a 5 μm phenyl LC column with an ammonium acetate, glacial acetic acid, acetonitrile, and water mobile phase. Eight blind duplicates of dietary supplements or botanicals were analyzed by 10 collaborators. Included was a negative control, ephedra nevadensis, and negative controls fortified at 2 different levels with each of the 6 ephedrine-type alkaloids. The spike levels were approximately 100 and 1000 μg/g for NE, 100 and 600 μg/g for NPE, 6500 and 65 000 μg/g for E, 1000 and 10 000 μg/g for PE, 300 and 3000 μg/g for ME, and 100 and 1000 μg/g for MPE. On the basis of the accuracy and precision results for this interlaboratory study, it is recommended that this method be adopted Official First Action for the determination of 6 different individual ephedrine-type alkaloids in dietary supplements and botanicals.

scholarly journals Rapid and Sensitive Method for Quantitative Determination of Lopinavir and Ritonavir in Human Plasma by Liquid Chromatography- Tandem Mass Specrtometry

2009 ◽  
Vol 6 (1) ◽  
pp. 223-230 ◽  
Author(s):  
G. A. Temghare ◽  
S. S. Shetye ◽  
S. S. Joshi
Keyword(s):  
Liquid Chromatography ◽  
Human Plasma ◽  
Solid Phase ◽  
Internal Standard ◽  
Therapeutic Monitoring ◽  
Tandem Mass ◽  
Limit Of Quantification ◽  
Liquid Chromatography Tandem Mass ◽  
Sensitive Method

A rapid and sensitive liquid chromatography-mass spectrometric (LC-MS-MS) method for the simultaneous determination of lopinavir and ritonavir in human plasma using abacavir as internal standard has been developed and validated. Sample preparation of plasma involved solid phase extraction. Detection was performed using an Applied Biosystems Sciex API 2000 Mass spectrometer. The assay of lopinavir and ritonavir was linear over the range of 50 ng mL-1to 20000 ng mL-1and 20 ng mL-1to 3000 ng mL-1 respectively with a precision of <15% and accuracy in the range of 85-115%. The limit of quantification in plasma for lopinavir and ritonavir was 50 ng mL-1and 20 ng mL-1respectively. The described method has the advantage of being rapid and easy and it could be applied in therapeutic monitoring of these drugs in human plasma

Determination of bosutinib in mice plasma and tissue by UPLC-MS/MS and its application to the pharmacokinetic and tissue distribution study

2015 ◽  
Vol 7 (21) ◽  
pp. 9184-9189 ◽  
Author(s):  
Linxia Wang ◽  
Luming Tang ◽  
Yi Zheng ◽  
Guoquan Pan ◽  
Wei Zhu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Internal Standard ◽  
Ultra Performance Liquid Chromatography ◽  
Tandem Mass ◽  
Distribution Study ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Tissue Distribution Study

A sensitive and rapid ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed to determine bosutinib in mice plasma and tissue using diazepam as the internal standard (IS).

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