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1.
Journal of Pharmaceutical Analysis ; (6): 92-99, 2011.
Article in Chinese | WPRIM | ID: wpr-686727

ABSTRACT

Monolithic silica spin column extraction (MonoSpin-SPE) was developed as a simple, sensitive, and eco-friendly pretreatment method which combined with ultra-fast liquid chromatography-mass spectrometry (UFLC-MS) to determine the levels of six phthalate esters, dimethyl- (DMP), diethyl- (DEP), dipropyl- [ DPrP], butyl-benzyl- (BBP), dicyclohexyl- (DcHP), and di-n-octyl-(DOP) phthalate in physiological saline samples. Under optimized experimental conditions, the method was linear in the following ranges: 0.2- 50 μg/L for DMP, DEP, DPrP, DcHP and DOP; 5- 100 μg/L for BBP. The correlation coefficients (R2 ) were in the range of 0. 9951 - 0. 9995 for all the analytes and the limits of detection (LODs) and limits of quantification (LOQs) were in the ranges of 0.02 - 0.9 μg/L and 0.08 - 2.7μg/L, respectively. The pretreatment process showed good reproducibility with inter-day and intra-day relative standard deviations (RSDs) below 8.5% and 11.2%, respectively. This method was used to determine the levels of six phthalate esters in physiological saline samples and the recoveries ranged from 71.2% to 107.3%. DMP and DEP were found in actual physical saline samples (brand A and brand B).

2.
Journal of Pharmaceutical Analysis ; (6): 92-99, 2011.
Article in Chinese | WPRIM | ID: wpr-474213

ABSTRACT

Monolithic silica spin column extraction (MonoSpin-SPE) was developed as a simple,sensitive,and eco-friendly pretreatment method which combined with ultra-fast liquid chromatography-mass spectrometry (UFLC-MS) to determine the levels of six phthalate esters,dimethyl-(DMP),diethyl-(DEP),dipropyl-[DPrP],butyl-benzyl-(BBP),dicyclohexyl(DcHP),and di-n-octyl-(DOP) phthalate in physiological saline samples.Under optimized experimental conditions,the method was linear in the following ranges:0.2 - 50 μg/L for DMP,DEP,DPrP,DcHP and DOP; 5- 100,μg/L for BBP.The correlation coefficients (R2 ) were in the range of 0.9951- 0.9995 for all the analytes and the limits of detection (LODs) and limits of quantification (LOQs) were in the ranges of 0.02- 0.9 μg/L and 0.08- 2.7 μg/L,respectively.The pretreatment process showed good reproducibility with inter-day and intra-day relative standard deviations (RSDs) below 8.5% and 11.2%,respectively.This method was used to determine the levels of six phthalate esters in physiological saline samples and the recoveries ranged from 71.2% to 107.3%.DMP and DEP were found in actual physical saline samples (brand A and brand B).

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