RESUMO
A UPCC-Q-TOF-MS method was established to analyze the components of polyoxyethylene 35 castor oil. The separation was performed at 50 ℃ on a Waters Acquity UPCC system by an Torus Diol column (3.0 mm × 100 mm, 1.7 μm) with gradient elution of CO2 and methanol - acetonitrile (50∶50); the flow rate was 1.0 mL·min-1, the back pressure was 2 000 psi, and methanol containing 2.5 mmol·L-1 ammonium formate was used as ionization reagent, whose flow rate was 0.2 mL·min-1. Positive ion electrospray ionization (ESI) mode and MSE technology were used. The qualitative analyses were carried out by using precise mass information of the parent and product ions and a PCA model was established by UPCC-Q-TOF-MS. L-02 cells and RBL-2H3 cells were used to study the cytotoxicity and histamine release of CrEL samples in vitro. A total of 13 kinds of CrEL components were obtained and their structures were identified by UPCC-Q-TOF-MS, with 255 compounds in total. The percentage content of 13 types of components was calculated by the normalization method. The content of polyoxyethylene glycerol tri-ricinoleate (PGTri-ricinoleate) in all samples was 0.36% - 2.80% and the main components were polyethylene glycol, polyethylene glycerol and polyoxyethylene glycerol mono-ricinoleate. All samples have different degrees of cytotoxicity and histamine release, which is negatively correlated with the content of PGTri-ricinoleate and positively correlated with the content of polyoxyethylene glycol fatty acid esters. The UPCC-Q-TOF-MS method is simple and rapid, has strong separation ability and high accuracy. It is suitable for the analysis of CrEL components. It is suggested that the fatty acid composition should be included in the monograph of CrEL for injection to increase the content of PGTri-ricinoleate and decrease the content of polyoxyethylene glycol fatty acid esters, so as to improve the product safety.
RESUMO
As one kind of lipid excipients, triacylglycerols (TAGs) are being more and more widely used in pharmaceutics with the development of advanced drug delivery systems. As their characteristics are mainly determined by their structures and compositions, strict quality control ought to be performed on TAGs, in order to guide their use in pharmaceutics. However, because of their complex compositions, no qualtity standard is set for TAGs in Ch.P currently. In this paper, we reviewed the methods for the separation and analysis of TAGs, includingthin-layer chromatog raphy, solid-phase extraction, gas chromotography, liquid chromatography, two-dimensional liquid chromatography, and ultraperformance convergence chromatography, and summarized their advantages and disadvantages. The application scope of each method was also overviewed in this review. Besides that we also pointed outthat according to our own study the newly emerged ultraperformance convergence chromatography would be one of the best methods to analyze TAGs.
RESUMO
OBJECTIVE: To develop a method suitable for rapid and accurate analysis of triacylglycerols in medium/long chain structured triacylglycerols by ultraperformance convergence chromatography combined with a quadrupole time-of-flight mass spectrometry. METHODS: The separation was performed at 28℃ on a Waters Acquity UPCC system by anHSS C18 SB column (3.0 mm×150 mm, 1.8 μm) with gradient elutionof CO2 and methanol acetonitrile (7:3, V/V), the flow rate was 1.2 mL·min-1, the back pressure was 117.2 MPa, and methanol containing 0.1% formic acid and 2 mmol·L-1 ammonium formate was used as supplement solvent. Positive ion electrospray ionisation (ESI) mode and MS technology were used in which two separate scan functions were programmed for the MS acquisition. The qualitative analyses were carried out by using precise mass information of parent ions and product ions. RESULTS: A total of 52 triacylglycerols were obtained and their stuctures were identified by analyzing the precise mass information of their parent ions and product ions respectively. CONCLUSION: The method is simple, highly accurate, and environmental friendly with good resolution, and can be used for rapid and accurate analysis of medium/long chain triacylglycerols excipients.