Optimization and Validation of HPTLC Method for Estimation of Ulipristal Acetate in Presence of Its Forced Degradation Products.

Ulipristal acetate (UPA) is used as emergency contraceptive and for uterine fibroids. No validated method has been reported to estimate UPA in presence of its degradation products. Therefore it is mandatory to develop method which can accurately measure it in presence of impurity. A simple and sensitive high-performance thin-layer chromatography (HPTLC) method was developed for the estimation of UPA. Pre-coated silica gel 60F254 TLC plates were as stationary phase and ethyl acetate:toluene:glacial acetic acid (4:7:0.3, v/v/v) was used as mobile phase. Drug was subjected to acid and alkali hydrolysis, oxidation, photo degradation and thermal degradation to study its degradation behavior. UPA eluted with Rf value 0.38 ± 0.02. The method was found to be linear in the concentration range of 400-3,600 ng/band. Limit of detection and limit of quantitation were found to be 72.7786 ng/band and 220.5412 ng/band, respectively. The % recovery of the proposed method was found to be 100.05-100.65%. The proposed method was specific to measure UPA in presence of degradants. The method was found to be accurate, precise, robust and can be useful for routine analysis of formulations containing UPA in presence of its degradation products.

Dispersive solvent-free ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction coupled with HPLC for determination of ulipristal acetate.

In this paper, a simple and efficient ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction (UA IL-DLLME) coupled with high-performance liquid chromatography for the analysis of ulipristal acetate (UPA) was developed. UPA could be easily migrated into 1-octyl-3-methylimidazolium hexafluorophosphate [C8mimPF6] IL phase without dispersive solvent. The research of extraction mechanism showed that hydrophobic interaction force played a key role in the IL-DLLME. Several important parameters affecting the extraction recovery were optimized. Under the optimized conditions, 25-fold enrichment factor was obtained and the limit of detection (LOD) was 6.8 ng mL(-1) (tablet) or 9.3 ng mL(-1) (serum) at a signal-to-noise ratio of 3. The calibration curve was linear over the range of 0.03-6.0 µg mL(-1). The proposed method was successfully applied to the UPA tablets and the real mice serum samples.

Progesterone receptors in breast cancer.

Sixty-six women who had received hormonal therapy for advanced disease were assessed for objective response to treatment. Another 51 patients who had received chemotherapy were similarly studied. Progesterone receptor was of no value as a predictor of patients unlikely to respond to hormone therapy, though it may have a role in predicting patients likely to respond favourably. The addition of progesterone receptor data to oestrogen receptor data may increase prediction of response in the ER+ range but clinicians should be cautious in their interpretation of progesterone receptor results in the ER- range. Progesterone receptor was of no value in predicting response to chemotherapy in this series. Analysis of survival data of 1731 women with primary breast cancer showed a highly significant trend toward longer survival in patients with progesterone receptor positive tumours than in those with receptor negative tumours (P less than 0.001). This trend was evident in both pre- and post-menopausal women. Even though the prognostic discrimination provided by progesterone receptor was correlated with that of oestrogen receptor, the addition of progesterone receptor data to oestrogen receptor data significantly improved prediction of survival (P less than 0.05).