PMID- 25240926 OWN - NLM STAT- MEDLINE DCOM- 20150527 LR - 20181202 IS - 1873-376X (Electronic) IS - 1570-0232 (Linking) VI - 970 DP - 2014 Nov 1 TI - Double-salting out assisted liquid-liquid extraction (SALLE) HPLC method for estimation of temozolomide from biological samples. PG - 86-94 LID - S1570-0232(14)00127-5 [pii] LID - 10.1016/j.jchromb.2014.02.031 [doi] AB - The role of temozolomide (TMZ) in treatment of high grade gliomas, melanomas and other malignancies is being defined by the current clinical developmental trials. Temozolomide belongs to the group of alkylating agents and is prescribed to patients suffering from most aggressive forms of brain tumors. The estimation techniques for temozolomide from the extracted plasma or biological samples includes high-performance liquid chromatography with UV detection (HPLC-UV), micellar electrokinetic capillary chromatography (MKEC) and liquid chromatography coupled to mass spectroscopy (LC-MS). These methods suffer from disadvantages like low resolution, low sensitivity, low recovery or cost involvement. An analytical method possessing capacity to estimate low quantities of TMZ in plasma samples with high extraction efficiency (%) and high resolution with cost effectiveness needs to be developed. Cost effective, robust and low plasma component interfering HPLC method using salting out liquid-liquid extraction (SALLE) technique was developed and validated for estimation of drug from plasma samples. The extraction efficiency (%) with conventional LLE technique with methanol, ethyl acetate, dichloromethane and acetonitrile was found to be 5.99+/-2.45, 45.39+/-4.56, 46.04+/-1.14 and 46.23+/-3.67 respectively. Extraction efficiency (%) improved with SALLE where sodium chloride was used as an electrolyte and was found to be 6.80+/-5.56, 52.01+/-3.13, 62.69+/-2.11 and 69.20+/-1.18 with methanol, ethyl acetate, dichloromethane and acetonitrile as organic solvent. Upon utilization of two salts for extraction (double salting liquid-liquid extraction) the extraction efficiency (%) was further improved and was twice of LLE. It was found that double salting liquid-liquid extraction technique yielded extraction efficiency (%) of 11.71+/-5.66, 55.62+/-3.44, 77.28+/-2.89 and 87.75+/-0.89. Hence a method based on double SALLE was developed for quantification of TMZ demonstrating linearity in the range of 0.47-20 mug/ml. The LOQ and LOD for the developed method were 0.4 mug/ml and 0.1 mug/ml, respectively. Thus, plasma non-interfering SALLE-HPLC method that is precise, robust, accurate, specific and cost effective for estimation of temozolomide from plasma samples was developed and validated. CI - Copyright (c) 2014 Elsevier B.V. All rights reserved. FAU - Jain, Darshana AU - Jain D AD - C.U. Shah College of Pharmacy, S.N.D.T. Women's University, Juhu Tara Road, Santacruz (West), Mumbai 400 049, India. FAU - Athawale, Rajani AU - Athawale R AD - C.U. Shah College of Pharmacy, S.N.D.T. Women's University, Juhu Tara Road, Santacruz (West), Mumbai 400 049, India. Electronic address: rajani.athawale@gmail.com. FAU - Bajaj, Amrita AU - Bajaj A AD - Dr. Bhanuben Nanavati College of Pharmacy, SVKM's, Vileparle, Mumbai 400 056, India. FAU - Shrikhande, Shruti AU - Shrikhande S AD - C.U. Shah College of Pharmacy, S.N.D.T. Women's University, Juhu Tara Road, Santacruz (West), Mumbai 400 049, India. LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20140228 PL - Netherlands TA - J Chromatogr B Analyt Technol Biomed Life Sci JT - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JID - 101139554 RN - 0 (Acetonitriles) RN - 0 (Sulfates) RN - 1K573LC5TV (potassium sulfate) RN - 451W47IQ8X (Sodium Chloride) RN - 7GR28W0FJI (Dacarbazine) RN - YF1K15M17Y (Temozolomide) RN - Z072SB282N (acetonitrile) SB - IM MH - Acetonitriles MH - Chromatography, High Pressure Liquid/*methods MH - Dacarbazine/*analogs & derivatives/blood/chemistry/isolation & purification MH - Humans MH - Linear Models MH - Liquid-Liquid Extraction/*methods MH - Reproducibility of Results MH - Sensitivity and Specificity MH - Sodium Chloride MH - Sulfates MH - Temozolomide OTO - NOTNLM OT - HPLC OT - SALLE OT - Salting out OT - Temozolomide OT - Validation EDAT- 2014/09/23 06:00 MHDA- 2015/05/28 06:00 CRDT- 2014/09/22 06:00 PHST- 2013/08/06 00:00 [received] PHST- 2014/02/06 00:00 [revised] PHST- 2014/02/18 00:00 [accepted] PHST- 2014/09/22 06:00 [entrez] PHST- 2014/09/23 06:00 [pubmed] PHST- 2015/05/28 06:00 [medline] AID - S1570-0232(14)00127-5 [pii] AID - 10.1016/j.jchromb.2014.02.031 [doi] PST - ppublish SO - J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Nov 1;970:86-94. doi: 10.1016/j.jchromb.2014.02.031. Epub 2014 Feb 28.