تعیین داروی سلکوکسیب با استفاده از روش میکرواستخراج فاز جامد پخشی جفت شده با اسپکتروفوتومتری فرابنفش - مرئی در نمونه های شیر، ادرار و آب

ﯾﮏ روش ﻣﯿﮑﺮواﺳﺘﺨﺮاج ﻓﺎز ﺟﺎﻣﺪ ﭘﺨﺸﯽ (dμspe )، آﺳﺎن و ارزان ﺟﻔﺖ ﺷﺪه ﺑﺎ اﺳﭙﮑﺘﺮوﻓﺘﻮﻣﺘﺮی ﻓﺮاﺑﻨﻔﺶ- ﻣﺮﺋﯽ ﺑﺮای اﻧﺪازه ﮔﯿﺮی ﺳﻠﮑﻮﮐﺴﯿﺐ در ﻧﻤﻮﻧﻪﻫﺎی ﺑﯿﻮﻟﻮژﯾﮑﯽ و آب ﺗﻮﺳﻌﻪ داده ﺷﺪ. ﺑﺮای اﯾﻦ ﻣﻨﻈﻮر، ﺟﺎذب ﺟﺪﯾﺪ ﻧﺎﻧﻮذرات ﻧﯿﮑﻞ دوپ ﺷﺪه در ﮔﺮاﻓﻦ اﮐﺴﯿﺪ ﮐﺮﺑﻮﮐﺴﯿﻞ دار ﺑﺎ اﺳﺘﻔﺎده از ﯾﮏ روش ﺷﯿﻤﯿﺎﯾﯽ ﺳﺎده ﺳﻨﺘﺰ و ﺑﺮای اﺳﺘﺨﺮاج ﺳﻠﮑﻮﮐﺴﯿﺐ از آن اﺳﺘﻔﺎده ﺷﺪ. ﻋﻮاﻣﻞ ﻣﻮﺛﺮ در اﺳﺘﺨﺮاج ﺑﺎ روش ﻃﺮاﺣﯽ آزﻣﺎﯾﺶ ارزﯾﺎﺑﯽ و ﺑﻬﯿﻨﻪ ﺳﺎزی ﺷﺪﻧﺪ. دو ﻃﺮح، ﺷﺎﻣﻞ ﻃﺮح plackett-burman و box-behnken ، ﺑﻪ ﺗﺮﺗﯿﺐ ﺑﺮای ﻏﺮﺑﺎﻟﮕﺮی و ﺑﻬﯿﻨﻪﺳﺎزی ﻋﻮاﻣﻞ ﻣﻮﺛﺮ ﻣﻮرد اﺳﺘﻔﺎده ﻗﺮار ﮔﺮﻓﺘﻨﺪ. اﯾﻦ روش در ﻣﺤﺪودة ﻏﻠﻈﺖ 0,004- 3,5 ﻣﯿﮑﺮوﮔﺮم ﺑﺮ ﻣﯿﻠﯽ ﻟﯿﺘﺮ ﺑﺎ 0.9951 = r2 ﺑﺮای اﻧﺪازهﮔﯿﺮی ﺳﻠﮑﻮﮐﺴﯿﺐ در ﺷﺮاﯾﻂ ﺑﻬﯿﻨﻪ ﺧﻄﯽ ﺑﻮد. ﺣﺪ ﮐﻤﯽ روش 0,004 ﻣﯿﮑﺮوﮔﺮم ﺑﺮ ﻣﯿﻠﯽ ﻟﯿﺘﺮ و ﻓﺎﮐﺘﻮر ﻏﻨﯽﺳﺎزی 21,7 ﺑﻮد. اﻧﺤﺮاف اﺳﺘﺎﻧﺪارد ﻧﺴﺒﯽ ﺑﺮای ﭘﻨﺞ اﻧﺪازهﮔﯿﺮی ﻣﺤﻠﻮل اﺳﺘﺎﻧﺪارد ﺳﻠﮑﻮﮐﺴﯿﺐ ﺑﺎ ﻏﻠﻈﺖ 0,3 ﻣﯿﮑﺮوﮔﺮم ﺑﺮ ﻣﯿﻠﯽ ﻟﯿﺘﺮ 3,2% ﻣﺤﺎﺳﺒﻪ ﺷﺪ. اﯾﻦ روش ﺑﺮای اﻧﺪازه ﮔﯿﺮی ﺳﻠﮑﻮﮐﺴﯿﺐ در ﻧﻤﻮﻧﻪﻫﺎی واﻗﻌﯽ ﺑﺎ ﺑﺎزﯾﺎﻓﺖ در ﻣﺤﺪودة 90,3- 96,8% و اﻧﺤﺮاف اﺳﺘﺎﻧﺪارد ﻧﺴﺒﯽ ﮐﻤﺘﺮ از 5,1 ﺑﺴﯿﺎر ﻣﻨﺎﺳﺐ اﺳﺖ. از ﻣﺰاﯾﺎی ﻣﻬﻢ اﯾﻦ روش ﻣﯽﺗﻮان ﺑﻪ ﺳﺎدﮔﯽ و ﺻﺮﻓﻪ اﻗﺘﺼﺎدی، ﻣﺼﺮف ﮐﻢ ﺣﻼل و ﺟﺎذب و ﻋﺪم ﻧﯿﺎز ﺑﻪ اﺑﺰار ﭘﯿﭽﯿﺪه و ﮔﺮان ﻗﯿﻤﺖ اﺷﺎره ﮐﺮد.

Determination of celecoxib with a dispersive micro solid-phase extraction coupled with UV-Vis spectrophotometric method in milk, urine and water samples

A sensitive, straightforward, and inexpensive dispersive micro solidphase extraction (DµSPE) coupled with the spectrophotometric method was developed for measuring celecoxib in biological and water samples. For this purpose, a new sorbent (Nickel nanoparticles doped carboxyl graphene oxide) was synthesized using a simple chemical procedure and was utilized to extract celecoxib. The effective factors in the DµSPE procedure were evaluated and optimized by the design of experiment method. Two designs, including the PlackettBurman design and BoxBehnken design, were applied to screening significant factors and to optimize the significant factors, respectively. The DµSPE spectrophotometric method was linear in the concentration range of 0.0043.5 µg mL1 with an Rsquared of 0.9951 for the celecoxib measurement under the optimum conditions. The method showed a low limit of detection of 0.004 µg mL1 and a suitable enrichment factor of 21.7 for the analyte determination. The relative standard deviation was calculated for five measurements of the standard solution of celecoxib with a concentration of 0.3 µg mL1 and was 3.2%. Finally, the proposed method was used to analyze real samples such as milk, urine, and tap water samples, indicating that the method is very suitable for measuring celecoxib in real samples with a recovery in the range of 90.396.8% with a relative standard deviation lower than 5.1 %. The important advantages of the method are simple and inexpensive procedure, low desorption solvent and sorbent consumption, and without the need for sophisticated and expensive instruments.