Determination Of Raloxifene Research Articles

Preparation of fluorescent sensor based on Zn metal-organic framework for detection and determination of raloxifene as an anticancer drug

Breast cancer is the second leading cause of death for women worldwide. Raloxifene (RLX) is a somewhat effective drug in lowering cholesterol, preventing and treating invasive breast cancer in postmenopausal women with osteoporosis, and does not interfere with breast tissue. Nevertheless, considering the possibility of risk in biological function due to excessive use of anticancer drugs and the adverse effects of drugs in wastewater on plants, animals, and aquatic, it is useful to determine the concentration of RLX in water and human body fluids. Here, a fluorescent metal-organic framework (MOF) nanoparticle based on trinuclear zinc clusters called Zn-MOF was presented, which is a high-performance and fast-response fluorescent chemosensor that can be used to detect RLX based on the fluorescence quenching medium in water. FTIR, XRD, SEM, and EDS analyses were used to identify the functional group and determine the structure and morphology of Zn-MOF. pH range 3–10. The prepared nanoparticles showed symmetric emission with excitation at a wavelength of 310.0 nm. The performance of the proposed fluorescent nanosensor was proportional to the quenching of the fluorescent signal with increasing RLX concentration at 404.0 nm; the quenching fluorescence response was linear in RLX concentration from 0.7 to 350 ng/mL with a significant detection limit equal to 0.485 nM.

Three-phase carrier-mediated hollow fiber microextraction based on deep eutectic solvent followed by HPLC–UV for determination of raloxifene and ethinylestradiol in pharmaceutical wastewater treatment plants

Endangering of the aquatic organisms and humans health by entrance of the pharmaceuticals in hydrosphere is becoming an important growing problem in the world. Effluents from wastewater treatment plants (WWTPs) are considered one of the main disposal pathways and incoming load of different pharmaceuticals in hydrosphere. In the present work, a new carrier-mediated hollow fiber liquid phase microextraction (CM-HFLPME) based on deep eutectic solvent (DES) was combined with HPLC–UV and applied for determination of ethinylestradiol (EE) and raloxifene (RLX) in pharmaceutical wastewater samples. The target analytes were extracted from 17 mL of the basic solution with pH 11 into an organic phase, as the supported liquid membrane (SLM) impregnated in the pores of a hollow fiber, and then back-extracted into the acceptor phase locating into the lumen of the hollow fiber. SLM consisted of n-octanol containing N,N,N-cetyltrimethyl ammonium bromide (CTAB), as the carrier, and the acceptor phase contained a mixture of DES and HCl. The important factors including sample pH, extraction time, HCl concentration and CTAB amount were optimized using a central composite design (CCD). Under the optimized conditions, preconcentration factors of RLX and EE were found to be 86 and 53, respectively. The limits of detections (LODs), based on 3S/N, were found to be 5.0 ng/mL for RLX and 10 ng/mL for EE, respectively. The calibration curves of RLX and EE were linear within the ranges of 20–5000 ng/mL (r2 = 0.9980) and 30–5000 ng/mL (r2 = 0.9985), respectively. Relative standard deviation (RSD%) of RLX and EE, based on three replicates at the concentration of 100 ng/mL, was calculated 1.7% and 2.6%, respectively. Finally, the feasibility of the proposed method was successfully confirmed by extraction and determination of RLX and EE in pharmaceutical wastewaters.

Development and Validation of a UPLC-MS/MS Assay for Simultaneous Estimation of Raloxifene and its Metabolites in Human Plasma

An aim of the study is development and validation of a method for the simultaneous estimation of raloxifene (RAL) and its two active metabolites, raloxifene-4-glucuronide (R4G) and raloxifene-6-glucuronide (R6G) in human plasma samples using raloxifene-D4 as an Internal Standard. Sample preparation was performed by solid phase extraction (SPE) and was followed by separation of the analytes on a UPLC system with a linear gradient and a mobile phase consisting of acetonitrile and ammonium formate. Detection was achieved by tandem mass spectrometry operated in the electrospray positive ion mode. The method had a short sample preparation time, as well as a chromatographic run time of just 4.2 min, the shortest so far reported for RAL, R4G and R6G determination. It was validated and fulfilled all preset criteria for sensitivity, specificity, linearity, within inter- and intra-accuracy and precision, stability studies for all molecules. The method was linear in the concentration range of 0.040 to 1.5 ng/mL, 0.6 to 50.0 ng/mL and 0.6 to 50.0 ng/mL for RAL, R4G and R6G, respectively. The proposed method could be applied to the rapid and reliable simultaneous determination of RAL, R4G and R6G in a bioequivalence study.

Determination of Raloxifene in Urine by Liquid Chromatography–Tandem Mass Spectrometry for Doping

Raloxifene is one of the selective estrogen receptor modulators and is often used to prevent and treat osteoporosis in postmenopausal women. Because of the indirect impact on serum testosterone levels and the potential ability for performance enhancement, it is banned by the World Anti-Doping Agency (WADA). This study established a fast, sensitive and selective liquid chromatography-tandem mass spectrometry method to quantify total raloxifene (unchanged and glucuronidated) in human urine for doping analysis. Urines from six healthy volunteers were collected 240 h after taking a single dose of raloxifene. The concentrations of urinary raloxifene were analyzed by the established method after sample preparation, including hydrolysis with β-glucuronidase. The lowest limit of quantification was 0.5 ng/mL. Linearity was observed for raloxifene concentrations ranging from 0.5 to 100 ng/mL, with a correlation coefficient of 0.999. The recoveries were >92.81%. Inaccuracies were below ±5%, and precisions varied from 2.18 to 5.37%. The results showed that urinary raloxifene was immediately detectable within 4 h after the administration of only a single dose of raloxifene. Such a result indicates a violation of the WADA rules. Furthermore, ingesting raloxifene would be detectable after 6 days in the urine of males or >10 days in the urine of female.

Resonance Rayleigh Scattering Method for the Determination of Raloxifene with Evans Blue

AbstractThe intensity of resonance Rayleigh scattering (RRS) of Evans blue (EB) or raloxifene hydrochloride (Ralo) is very weak, but it can be enhanced significantly and a new RRS spectrum appears when both of them interact to form an ion‐association complex in sodium acetate‐hydrochloric acid buffer solution at pH 1.8. The intensity of RRS is directly proportional to the concentration of Ralo in the range of 0–8.3 μg · mL−1, and the detection limit for Ralo (σ = 3) is 18.9 ng·mL−1. The method has high sensitivity and fairly good selectivity. Based on the above evidences, a new facile method for the determination of trace amount of Ralo has been established with satisfactory results.