Semi‐micro column high‐performance liquid chromatography with UV detection for quantification of aspirin and salicylic acid and its application to patients' sera administered with low‐dose enteric‐coated aspirin

Abstract

A simultaneous determination of aspirin (ASA) and its metabolite, salicylic acid (SA), in human serum by a semi-micro column HPLC-UV was developed. A relatively small size of serum sample (100 microL) containing ASA and SA was cleaned up by a simple solid phase extraction. A good separation of ASA and SA could be achieved within 25 min using a semi-micro ODS column with an eluent of MeOH/0.7 mm phosphoric acid solution (pH 2.5) = 50:50 (v/v). The calibration curves for ASA and SA showed good linearity (r = 0.999) with the detection limits 114 and 38 ng/mL at a signal-to-noise ratio of 3, respectively. ASA and SA in patients' sera administered with low-dose enteric-coated aspirin were determined, and the concentration ranges obtained for ASA and SA were 1.2-2.2 and 0.5-57.3 microg/mL, respectively.

Optimization of microwave‐assisted extraction of analgesic and anti‐inflammatory drugs from human plasma and urine using response surface experimental designs†

“…The LODs achieved ranged from 4 to 45 ng/mL for plasma and from 8 to 85 ng/mL for urine (Table ). The results indicate that the proposed MAE‐HPLC‐PDA method is suitable for the determination of trace NSAIDs and provides limits of detection lower than those obtained when SPE (for salicylic acid, acetaminophen, diclofenac, and ibuprofen) was applied to plasma and water samples , and for metamizol and tramadol in analgesic mixture solutions . Therefore, LODs are similar than those achieved for salicylic acid and diclofenac using phosphoric acid to disrupt such drug‐protein binding before LC‐MS and for diclofenac after LLE and HPLC with electrochemical detection .…”

Development and Application of Sensitive Methods with Luminescence Detections for Determination of Biologically Active Compounds

“…These compounds in patients' sera administered with low-dose entericcoated aspirin were determined, and the concentration ranges obtained for aspirin and salicylic acid were 1.2-2.2 and 0.5-57.3 µg/ml, respectively. 22) Mildly to severely elevated plasma concentrations of homocystein (HCY) are positively associated with an increased risk of atherosclerosis, independent of traditional vascular disease risk factors. The determinants of HCY and carotid intimamedia thickness, a clinical marker for the detection of atherosclerosis in Japanese were evaluated.…”

Determination of Salicylic Acid in Human Serum and Urine Samples by High-Performance Liquid Chromatography with Post-column Ru(bipy)32+-Ce(SO4)2 Chemiluminescence Detection

“…A variety of methods are available for the determination of SA, including spectrophotometry 1 (detection limit, DL, 5.952 × 10 -6 g/mL), flow-injection analytical atomic absorption spectrometery (FIA-AAS) 2 and high-performance liquid chromatography (HPLC) [3][4][5]9 (DL = 3.8 × 10 -8 g/mL); Although UV detection cannot be used to achieve low detection limits, MS 6,7 detection (DL = 1.5 × 10 -8 g/mL) and FL 8 detection (DL = 1.38 × 10 -9 g/mL) can achieve low detection limits for applications to pharmaceutical samples. The chemiluminescence (CL) method [10][11][12][13] was also reported for the determination of SA, but its application was limited due to lower selectivity, or a high concentration of an acidic medium, which was corrosive to the flow-type experimental system, or the need for a complex procedure and special handling technique when preparing the reactor.…”