“…The product ion at m/z 227 was formed by the neutral loss of 2-amino-4-phenylbutanoic acid (179 Da). The CID spectrum of protonated lisinopril was similar to those obtained in previous studies (Burinsky and Sides, 2004;Pei et al, 2006).…”
Section: Identification Of the Unknown Impuritiessupporting
Two trace impurities in the bulk drug lisinopril were detected by means of high-performance liquid chromatography coupled with mass spectrometry (HPLC/MS) with a simple and sensitive method suitable for HPLC/MS n analysis. The fragmentation behavior of lisinopril and the impurities was investigated, and two unknown impurities were elucidated as 2-(6-amino-1-(1-carboxyethylamino)-1-oxohexan-2-ylamino)-4-phenylbutanoic acid and 6-amino-2-(1-carboxy-3-phenylpropylamino)-hexanoic acid on the basis of the multi-stage mass spectrometry and exact mass evidence. The proposed structures of the two unknown impurities were further confirmed by nuclear magnetic resonance (NMR) experiments after preparative isolation.
“…The product ion at m/z 227 was formed by the neutral loss of 2-amino-4-phenylbutanoic acid (179 Da). The CID spectrum of protonated lisinopril was similar to those obtained in previous studies (Burinsky and Sides, 2004;Pei et al, 2006).…”
Section: Identification Of the Unknown Impuritiessupporting
Two trace impurities in the bulk drug lisinopril were detected by means of high-performance liquid chromatography coupled with mass spectrometry (HPLC/MS) with a simple and sensitive method suitable for HPLC/MS n analysis. The fragmentation behavior of lisinopril and the impurities was investigated, and two unknown impurities were elucidated as 2-(6-amino-1-(1-carboxyethylamino)-1-oxohexan-2-ylamino)-4-phenylbutanoic acid and 6-amino-2-(1-carboxy-3-phenylpropylamino)-hexanoic acid on the basis of the multi-stage mass spectrometry and exact mass evidence. The proposed structures of the two unknown impurities were further confirmed by nuclear magnetic resonance (NMR) experiments after preparative isolation.
“…Spectroscopic [8][9][10], High Performance Liquid Chromatography (HPLC) [11][12][13], Thin Layer Chromatography (TLC) [14], Electrochemical [15][16][17] and mass spectrometry [18] methods for estimation of MOX alone or in combination with other drugs in pharmaceutical preparation have been reported. Hydrochlorothiazide alone or in combination with other drugs is estimated by HPLC [19][20][21][22][23][24][25][26][27][28][29], TLC-densitometry [30][31][32][33][34][35][36], capillary electrophoresis [37][38][39], electrochemical [40][41][42][43] and spectroscopic methods [44][45][46][47][48][49][50][51][52][53].…”
Section: Moexipril Hydrochloride (Mox) Is Chemically (3s)-2-[(2s)-2-{mentioning
In this study determination of Moexipril hydrochloride (MOX) and hydrochlorothiazide (HCT) were conducted by application of Spectrophotometric and Chemometric methods. Five different accurate, sensitive and reproducible methods were applied for the simultaneous determination of (MOX) and (HCT) in their bulk powder and pharmaceutical dosage form. The first method is the new absorbance subtraction (AS) method. The second method is the new amplitude modulation (AM) method. The third method is the new extended ratio subtraction (ERS) method coupled to ratio subtraction (RS) method. The fourth and fifth methods are multivariate calibration which includes Principal Component Regression (PCR) and Partial Least Squares (PLS). The suggested procedures were checked using laboratory prepared mixtures and were successfully applied for the analysis of their pharmaceutical preparations. The validity of the proposed methods was further assessed by applying the standard addition technique. The results obtained by applying the proposed methods were statistically analyzed and compared with a reported method.
“…wts. and fragmentation scheme of the two wellknown degradation products of the drug [1,16], which were also listed in EP [15], viz., enalaprilat and diketopiperazine derivative, respectively. The m/z value of peak III matched to the mol.…”
Section: Lc-ms Studies On Forced Decomposition Samples Of Enalapril Mmentioning
confidence: 99%
“…5 gives the proposed scheme of fragmentation of the drug, and products I, II (enalaprilat) and III. The fragmentation pattern for drug and II is based on the behavior reported by Burinsky and Sides [16]. One major fragmentation route for these molecules includes elimination of ethylformate from enalapril and formic acid from II, to yield a common fragment of m/z 303, which does not seemingly fragments further.…”
Section: Lc-ms Studies On Forced Decomposition Samples Of Enalapril Mmentioning
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