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Article
Preparation and Study of Cephalexin Selective Electrodes and Their Application in Pharmaceutical Drugs

Author: Khaleda H. Al-Saidi
Journal: Al-Mustansiriyah Journal of Science مجلة علوم المستنصرية ISSN: 1814635X Year: 2010 Volume: 21 Issue: 6 Pages: 179-191
Publisher: Al-Mustansyriah University الجامعة المستنصرية

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Abstract

A plastic membrane electrodes for the determination of cephalexin monohydrate were fabricated based on the use of cephaiexin-phosphotungstate as an active substance, and with different plasticizers, di-butyl phosphate (DBP), di-butyl phthalate (DBPH), di-octyl phthalate (DOP), tri-butyl phosphate (TBP) and o-nitro phenyl octyl ether (NPOE) in PVC matrix membranes. The study was carried out to investigate the electrode parameters, effect of pH and selectivity. Internal filling solution of 10-3 M Ceph + 10-3 M NaCl was used to fill the electrodes. The best electrodes were based on DBPH and DOP plasticizer which gave a slope 59.5 and 58.5 mV/decade, linear concentration range 10-4 – 10-2 M and detection limit of 5 x 10-5 and 3 x 10-5 M, respectively displayed good stability and reproducibility. The electrodes were used to determine the cephalexin monohydrate in oral suspension and capsules, the average recovery and standard deviation were (100.116 ± 0.393) and (100.344 ± 0.120), respectively. The results were compared with UV-derivative spectrophotometry (DS) and the results for the drugs obtained by first derivative are quite comparable with the recovery obtained by cephalexin selective electrodes.

حضرت أقطاب ﺇنتقائية للسيفاتكسين بتحضير المادة الفعالة (السيفالكسين- فوسفوتنكستيت) Ceph-PT مع الملدنات المختلفة وهي داي بيوتيل فوسفيت (DBP) , داي بيوتيل فثاليت (DBPH) ,داي اوكتيل فثاليت (DOP) ,ثراي بيوتيل فوسفيت (TBP) و اورثو نيترو فنيل ﺇيثر (NPOE) في غشاء اصله من بولي فاينيل كلورايد .(PVC) الدراسة شملت خواص ألأقطاب كتأثير الدالة الحامضية ( pH ) ، المحلول الداخلي للأقطاب, الأنتقائية وحد التحسس ومدى الخطية . ﺇن أفضل الأقطاب المحضرة هي باستعمال الملدنات ((DBPH, DOP. والمحلول الداخلي (10-3M Ceph+10-3M NaCl) حيث ان الميل لمنحني المعايرة هو ( (59.5و58.5mV/decade وبحدود تحسس( 5x10-5 , 3x10-5 M) على التوالي و مدى خطية متساوي 10-4 – 10-2 M ولهما ثبوتية وتكرارية جيدة. ﺇن هذه الأقطاب أستخدمت لتقدير السيفالكسين في المستحضرات الدوائية الكبسول والمعلق الفموي وان معدل الأسترجاع والانحراف المعياري كالأتي : (100.116 ± 0.393) (100.344) ± 0.120) ,. تمت مقارنة النتائج المستحصلة من الأقطاب مع نتائج المشتقات الطيفية حيت تطابقت نتائج المشتقة الطيفية الأولى من حيث قيمة نسبة الاسترجاع والدقة وسهولة الطريقة.

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Article
Preparation and Potentiometric Study of Amiloride Hydrochloride Selective Electrodes and Their Application in Determining Some Drugs

Author: Khaleda, H. Al-Saidi
Journal: Al-Mustansiriyah Journal of Science مجلة علوم المستنصرية ISSN: 1814635X Year: 2010 Volume: 21 Issue: 6 Pages: 212-229
Publisher: Al-Mustansyriah University الجامعة المستنصرية

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Abstract

Amiloride hydrochloride ion-selective electrodes were constructed in polymeric membrane by using PVC and based on the use of active ion-pair (Amiloride-phosphotungstate) and the other ion pair (Amiloride- tetraphenyl -borate). The plasticizers used were Di-butyl phthalate (DBPH), Di-octylphthalate (DOP) and Tri-butyl phosphate (TBP). The electrodes (A, B and C) based on the ion pair (Amiloride -phosphotungstic acid) and (D, E and F) based on the ion pair (Amiloride - tetraphenylborate) and the plasticizers used DBPH, DOP and TBP respectively they gave approximately the same linear concentration range from (1x10-5 to 1x10-2) M. The slopes are (54.198, 52.759, 50.910, 49.007, 48.508 and 48.501) mV/decade, and the detection limit were (6×10-7, 1.5×10-6, 7×10-6 , 1.75×10-5, 7×10-6 and 1.5×10-5)M, with the response time (10, 30, 10, 12, 10 and 35) Sec. and the lifetime were about (45, 35, 30, 21, 15 and 10) days respectively. And the working pH range found to be (1.9 –7.8) for the concentration of Amiloride solution 1×10-3 M by using electrode A (Amilo-PT+DBPH). The measurement interferences in the presence of Na+, K+, Mg2+, Mn2+, Cu2+, , Fe3+ and Hydroclorothiazide were studied using separate and mixed methods for selectivity coefficient determination. The pH and life time of the electrodes were also studied. The analytical methods results showed to be simple, rapid and with a good accuracy by comparing it with UV-spectrophotometric method by using F-test.

تم تصنيع عدة أقطاب پوليمريه من مادة الپولي ڤاينايل كلورايد حساسة للاميلورايد هيدروكلورايد بالاعتماد على المعقد المحضر (Amiloride-phosphotungistate ) والمعقد الثاني (Amiloride-tetraphenylborate) كمادة فعالة. هذه المادة الفعالة تكون مذابة في عدة مواد ملدنه منها :Di-butylphthalate (DBPH), Di-octylphthalate (DOP), Tri-butyl phosphate (TBP), وقد تم دراسة خواص هذه الأقطاب و التي شملت(ميل منحني المعايرة و معامل الارتباط و مدى التراكيز و حد التحسس و عمر القطب (ومن خلال الدراسة ٲظهرت النتائج ٲن ٲقطاب الاميلورايد:Amilo-PT+DBPH, Amilo-PT+DOP, Amilo-PT+TBP, Amilo-TPB+ DBPH, Amilo-TPB + DOP, Amilo-TPB +TBP,لها تقريبا نفس مدى التركيز الخطي 1x10-5 1x10-2 – مولاري وإنحدار54.198, 48.501,48.508,49.007 ,50.91,52.759 ملفولت/حقبة على التوالي. و حد التحسس (1.5×10-5 ,7×10-6, 6×10-7, 1.5×10-6, 7×10-6 ,1.75×10-5) مولاري, زمن الإستجابة ( 35, 10, 12 10, 30, 10) ثانية للتركيز 10-3 مولاري و عمر القطب (45, 35, 30, 21 , 15, 10) يوم على التوالي. و مدى الدالة الحامضية وجد بحدود(1.9 – 7.8) لتركيز محلول الاميلورايد 10-3 مولاري باستخدم القطب (A) .Amilo-PT+DBPHأيضاً درست التداخلات لبعض الأيونات الاحادية والثنائية والثلاثية و تداخل نوع ﺁخر من الادوية المدررة مثل الهايدوكلوروثايازايد بوساطة طريقة المحاليل المنفصلة وطريقة المحاليل الممزوجة لتعين معامل الانتقائية (potA,BK) و كذلك استخدم القطب (A) في التقدبرات الإجهادية لتعين الاميلورايد في الأدوية التجارية و اظهرت النتائج بأن الطريقة المستخدمة بسيطة, سريعة و دقيقة مقارنةً بطريقة الاطياف .

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Article
SIMULTANEOUS DETERMINATION OF AMILORIDE HYDROCHLORIDE AND HYDROCHLOROTHIAZIDE IN PHARMACEUTICALS BY DERIVATIVE SPECTROPHOTOMETRY

Authors: Khaleda, H. Al-Saidi --- Suhad Abdlaziz --- Sahar Semer
Journal: Al-Nahrain Journal of Science مجلة النهرين للعلوم ISSN: (print)26635453,(online)26635461 Year: 2010 Volume: 13 Issue: 4 Pages: 52-61
Publisher: Al-Nahrain University جامعة النهرين

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Abstract

Method is established for simultaneous determination of Amiloride hydrochloride (Amilo) andhydrochlorothiazide in tablets. The method is based on employing normal and derivativespectrophotometry using the zero order via described by measuring the absorbance at 361 nm andthe first order derivative spectra at peak 340 and valley 382 nm for (Amilo), while the zerocrossingmethod is applied for hydrochlorothiazide. The first order derivative absorption spectra atvalleys 285 and 239 nm were used for hydrochlorothiazide. No interferences found betweenboth determined and those of matrices. A good accuracy and precision of simultaneousdetermination of (Amilo), and hydrochlorothiazide were confirmed by statistical analysis. Thepercentage recovery of the individual drags under the established conditions is ranged from 97.79%to 101.5 %. Linearity is maintained within a wide concentration range from 2.00 mg/L to 40.00mg/L for Amiloride hydrochloride and hydrochlorothiazide. The detection limit was 0.5 and 1.0mg/L for Amiloride hydrochloride and hydrochlorothiazide respectively.


Article
Simultaneous determination of paracetamol and cephalexin binary mixtures by using derivative spectrophotometry and H-point standard addition methods

Authors: Asraa A. Al-Abaas --- Firyal Waly Askar --- Khaleda, H. Al-saidi
Journal: Journal of College of Education مجلة كلية التربية ISSN: 18120380 Year: 2010 Issue: 1 Pages: 43-58
Publisher: Al-Mustansyriah University الجامعة المستنصرية

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Abstract

Two methods are applied for simultaneous determination of paracetamol (para) and cephalexin (ceph) in combined mixtures, derivative spectrophotometric technique and H-Point standard addition method (HPSAM) spectrophotometry. The first procedure is based on the use of the, second derivative ( 2D ) and used the suitable wave lengths at zero crossing at valley 250.5 and 290.2 nm for determination paracetamol and cephalexin respectively.. Calibration graphs were established for 2-60 mg/L for Para and 2-70 mg/L for ceph in binary mixture. The proposed method were successfully applied to the determination of these drugs in synthetic mixtures, linearity was excellent (r2>0.999) over the concentration tested (2–60 mg/L) with good precision and accuracy. Recoveries were good (>98%) with limits of detection of 1 and 1.5 mg/L ,(%R.S.D.= 0.757- 1.207) for para and ceph, respectively.. The second procedure HPSAM was applied to the simultaneous determination of Para and ceph. respectively. (HPSAM) method was based on the difference in the absorbance of para and ceph.at choosing wavelengths (265 and 257 nm). Results of the analysis of the different mixtures in the proposed system revealed a dynamic range of 2-35 and 2-50 mg/L, with limits of detection of 2 and 3 mg/L for para and ceph, respectively. The relative error are between -0.605-1.64 and -1.230-1.43, for para and ceph respectively. RSD% 0.151-1.775 for para and ceph, respectively. The two methods were found to be precise, accurate, simple and rapid..

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