Rapid quantification of lisinopril in human plasma by liquid chromatography/tandem mass spectrometry

Abstract

An assay based on protein precipitation and liquid chromatography/tandem mass spectrometry (LC-MS/MS) has been developed and validated for the quantitative analysis of lisinopril in human plasma. After the addition of enalaprilat as internal standard (IS), plasma samples were prepared by one-step protein precipitation using perchloric acid followed by an isocratic elution with 10 mm ammonium acetate buffer (pH adjusted to 5.0 with acetic acid)-methanol (70:30, v/v) on a Phenomenex Luna 5 mu C(18) (2) column. Detection was performed on a triple-quadrupole mass spectrometer utilizing an electrospray ionization (ESI) interface operating in positive ion and selected reaction monitoring (SRM) mode with the precursor to product ion transitions m/z 406 --> 246 for lisinopril and m/z 349 --> 206 for enalaprilat. Calibration curves of lisinopril in human plasma were linear (r = 0.9973-0.9998) over the concentration range 2-200 ng/mL with acceptable accuracy and precision. The limit of detection and lower limit of quantification in human plasma were 1 and 2 ng/mL, respectively. The validated LC-MS/MS method has been successfully applied to a preliminary pharmacokinetic study of lisinopril in Chinese healthy male volunteers.

Quantitative determination of lisinopril in human plasma by high performance liquid chromatography–tandem mass spectrometry and its application in a pharmacokinetic study

“…The extraction recoveries from QC samples at low, mid and high concentrations were 81.5 ± 6.0, 87.2 ± 1.7 and 86.0 ± 5.3% for lisinopril, and 84.9 ± 8.4% for IS. The recoveries were much higher than the values reported in the literature (Kousoulos et al , ; Padua et al , ; Qin et al , ; Sagirli et al , 2004; Wong et al , 1995). In terms of matrix effect, all the ratios defined in the Experimental were between 85 and 115%.…”

“…Typical equations for the calibration curves were: y = 1.32 × 10 −2 x + 1.35 × 10 −3 , r = 0.998. The LLOQ for lisinopril was 1.03 ng/mL in plasma, which was lower than the values reported in the literature (Kousoulos et al , ; Padua et al , ; Qin et al , ; Tashtoush et al , ; Tsakalof et al , ; Zhou et al , ).…”

“…Finally, a mobile phase consisting of methanol–water containing 0.2% formic acid (55:45, v/v) was used. Under the optimal conditions, the total run time for each sample was only 2.5 min, which was shorter than the values (3.5–10 min) reported for HPLC/MS methods in the literature (Huang et al , ; Padua et al , ; Qin et al , ; Tashtoush et al , ; Tsakalof et al , ; Zhou et al , ).…”

“…This paper describes an improved, rapid, selective and sensitive HPLC‐MS/MS method that enables the determination of lisinopril with good accuracy at low drug concentrations in human plasma. The lower limit of quantification (LLOQ) was 1.03 ng/mL, which was lower than that reported in the literature (Kousoulos et al , ; Padua et al , ; Qin et al , ; Tashtoush et al , ; Tsakalof et al , ; Zhou et al , ). The total run time of the method per sample was 2.5 min, which was shorter than reported values (Huang et al , ; Padua et al , ; Qin et al , ; Tashtoush et al , ; Tsakalof et al , ; Zhou et al , ).…”

“…During recent years, liquid chromatography–mass spectrometry, LC‐MS/MS (Huang et al , ; Padua et al , ; Qin et al , ) and LC‐MS (Tashtoush et al , ; Tsakalof et al , ; Zhou et al , ) have been used in the determination of lisinopril. However, these methods need long analysis times (>3.5 min) or complicated and time‐consuming sample pretreatment procedures, which do not meet the requirement for high throughput and speed in biosample analysis.…”