Development and validation of a reversed-phase HPLC method for the determination of lisinopril and gliclazide in pharmaceuticals

Abstract

The aim of the present study was to develop and validate a

High-Performance Liquid Chromatography (HPLC) method

for the determination of lisinopril and gliclazide. The method

was developed on Zorbax C8 analytical column (4.6x250 mm;

5μm) by isocratic elution with a flow rate of 1.0 mL/min and

injection volume of 25 μl. The mobile phase composition was

methanol:water (65:35 v/v, pH adjusted to 3.0 triethylamineorthophosphoric

acid buffer) and the retention time was

found to be 2.883 and 7.456 min for lisinopril and gliclazide,

respectively. The developed method was found to be linear in

the concentration range of 5-20 μg/mL for lisinopril and 15-60

μg/mL for gliclazide. The method was validated for linearity,

accuracy, precision, LOD and LOQ. This developed procedure

was succesfully applied conveniently for the analysis of lisinopril

and gliclazide in pharmaceutical preparations.

Keywords

• Combined dosage forms,gliclazide,lisinopril,RPHPLC,method validation

Farmasötik ürünlerde lisinopril ve gliklazid tayini için ters faz-yüksek basınçlı sıvı kromatografisi yönteminin geliştirilmesi ve validasyonu

Abstract

Mevcut çalışmanın amacı, lisinopril ve gliklazid etken maddeleri

için yüksek performanslı sıvı kromatografisi kullanılarak

bir analitik yöntemin geliştirilmesi ve validasyonunu

kapsamaktadır. İzokratik ayırım ile sağlanan bu yöntem, 25

mikrolitre enjeksiyon hacmi ve 1.0 mL/dk’ya akış hızı ile

Zorbax C8 analitik kolon (4.6x250 mm; 5μm) kullanılarak

geliştirilmiştir. Hareketli faz bileşimi metanol:su içermekte olup

(65:35 v/v, pH=3’e trietilamin-ortofosfat tamponu ile ayarlı)

lisinopril ve gliklazid için alıkonma zamanı sırasıyla 2.883 ve

7.456 dk. olarak bulunmuştur. Geliştirilen bu yöntem lisinopril

için 5-20 μg/mL konsantrasyon aralığında, gliklazid için ise

15-60 μg/mL konsantrasyon aralığında doğrusaldır. Yöntem

doğrusallık, kesinlik, doğruluk ve LOD-LOQ validasyon

parametreleri açısından valide edilmiştir. Geliştirilen bu

prosedür lisinopril ve gliklazidin farmasötik preparatlarının

analizlerinde güvenli bir şekilde uygulanabilir.

Keywords

• Kombine dozaj formu,gliklazid,lisinopril,ters faz-HPLC,yöntem geliştirme

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