HPLC determination of cisatracurium besylate and propofol mixtures with LC-MS identification of degradation products

Zhang, H; Wang, P; Bartlett, Michael G.; Stewart, James T.

doi:10.1016/s0731-7085(97)00262-8

Cited by 28 publications

(16 citation statements)

References 13 publications

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“…Propofol was much less sensitively ionized in the positive ion mode than in the negative ion mode by either°APCI°or°ESI° [15].°Similarly°none°of°the°other phenols used in this study was ionized efficiently in the positive ion mode. At typical working concentrations of 500 ng/ml used in this study the positive ion mode did not produce a detectable ion signal.…”

Section: Positive Ion Studymentioning

confidence: 66%

“…One report on the fragmentation of phenolic anions in the gas phase is restricted to phenol only [12]. Reports on negative ion LC/MS for the identification of propofol using APCI for ionization fail to discuss its fragmentation [15,16]. Fragmentation of the [M ϩ H] ϩ ion of sterically hindered phenols formed by chemical ionization using methane or butane as the reagent gas [17,18] indicate the formation of product ions by the loss of a methyl radical at the ␤ carbon of substituent side chains.…”

Section: The Presence Of the Intermediary [M ϫ H ϫ Ch 3 ]mentioning

confidence: 99%

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Mass spectral fragmentation of the intravenous anesthetic propofol and structurally related phenols

Bajpai

Varshney

Seubert

et al. 2005

J. Am. Soc. Mass Spectrom.

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Propofol (2,6-diisopropyl phenol) is a widely used intravenous anesthetic. To define its pharmacokinetics and pharmacodynamics, methods for its quantitation in biological matrixes have been developed, but its pattern of mass spectral fragmentation is unknown. We found that fragmentation of the [M Ϫ H] Ϫ ion (m/z 177) of propofol in both APCI MS/MS and ESI MS/MS involves the stepwise loss of a methyl radical and a hydrogen radical from one isopropyl side chain to give the most intense product ion, [M ϪH Ϫ CH 4 ] Ϫ , at m/z 161. This two-step process is also the preferred mode of fragmentation for similar branched alkyl substituted phenols. This mode of fragmentation of the [M Ϫ H] Ϫ ion is supported by three independent lines of evidence: (1) Ϫ product ion. Phenols with a single straight chain alkyl substituent, in contrast, undergo ␤ elimination of the alkyl radical irrespective of the length of the alkyl chain, yielding the most intense product ion at m/z 106. This product ion represents a special case of a stable intermediary radical for the two-step process described for branched side chains, because further elimination of a hydrogen radical from the ␤ carbon is not possible. as a supplement to regional anesthesia and in critically ill patients confined to intensive care units. The patient loses consciousness 30 to 50 s after receiving the drug and remains asleep for about 4 to 6 min [1,2]. Even though a single dose of propofol has a short duration of action and produces fast recovery from anesthesia, propofol is not metabolized in a few minutes. It is present in blood, adipose tissues, liver, and brain for a few hours, its concentration decreasing with time [4].

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Section: Positive Ion Studymentioning

confidence: 66%

Section: The Presence Of the Intermediary [M ϫ H ϫ Ch 3 ]mentioning

confidence: 99%

Mass spectral fragmentation of the intravenous anesthetic propofol and structurally related phenols

Bajpai

Varshney

Seubert

et al. 2005

J. Am. Soc. Mass Spectrom.

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“…Os reagentes utilizados no procedimento analítico apresentaram grau de Vários métodos têm sido descritos na literatura para a análise das concentrações plasmáticas de propofol utilizando cromatografia líquida de alta eficiência com detecção ultravioleta (UV) (KNIBBE et al, 1998;ZHANG et al, 1998;EMARA et al, 1999), fluorescência (CHAN et al, 1990;EL-YAZIGI et al, 1996;YEGANCH et al, 1997) ou eletroquímico (DOWRIE et al, 1996), e também utilizando cromatografia a gás com detector de massas (STETSON et al, 1993).…”

Section: Reagentes Padrões De Referência E Soluçõesunclassified

Avaliação da função pulmonar em pacientes submetidos à cirurgia cardíaca com circulação extracorpórea

Barbosa¹

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“…Co‐administration of PPF with CAC is frequently employed throughout surgery as a preoperative practice . A literature survey revealed that few research articles have reported the determination of a combination of PPF and CAC relying on the use of HPLC . Therefore, there is still a need for a more simple, sensitive and fast alternative method for the simultaneous estimation of both drugs in human plasma.…”

Section: Introductionmentioning

confidence: 99%

First derivative synchronous spectrofluorimetric method for the simultaneous determination of propofol and cisatracurium besylate in biological fluids

et al. 2019

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Propofol and cisatracurium besylate have been simultaneously determined using a highly sensitive first derivative synchronous spectrofluorometric method. The method is based on measuring first derivative synchronous spectrofluorimetric amplitude at Δλ = 40 nm with a scanning rate of 600 nm/min. The different experimental parameters affecting the fluorescence intensity of the two drugs were carefully studied and optimized. The amplitude–concentration plots were rectilinear over the range 40.0–400.0 ng/mL and 20.0–280.0 ng/mL for propofol and cisatracurium, respectively with lower detection limits of 4.0 and 2.35 ng/mL and quantification limits of 12.1 and 7.1 ng/mL for propofol and cisatracurium, respectively. The proposed method was successfully applied for the determination of the two compounds in synthetic mixtures and in commercial ampoules. The high sensitivity attained using the proposed method allowed the simultaneous determination of both drugs in spiked plasma samples. The mean % recoveries in spiked human plasma (n = 3) were 96.53 ± 0.90 and 96.20 ± 1.64 for each of propofol and cisatracurium, respectively. The method was validated in compliance with International Council of Harmonization (ICH) Guidelines.

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HPLC determination of cisatracurium besylate and propofol mixtures with LC-MS identification of degradation products

Cited by 28 publications

References 13 publications

Mass spectral fragmentation of the intravenous anesthetic propofol and structurally related phenols

Mass spectral fragmentation of the intravenous anesthetic propofol and structurally related phenols

Avaliação da função pulmonar em pacientes submetidos à cirurgia cardíaca com circulação extracorpórea

First derivative synchronous spectrofluorimetric method for the simultaneous determination of propofol and cisatracurium besylate in biological fluids

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