Validated Reverse Phase-High-Performance Liquid Chromatography Method for Estimation of Fisetin in Self-Nanoemulsifying Drug Delivery System
Rajan KumarRakesh KumarRubiya KhursheedAnkit AwasthiArya Kadukkattil RamanunnyJaskiran KaurNavneet KhuranaSachin Kumar SinghShelly KhuranaNarendra Kumar PandeyBhupinder KapoorNeha Sharma
14
Citation
23
Reference
10
Related Paper
Citation Trend
Abstract:
Fisetin (FS) is a polyphenolic phytoconstituent reported to have various pharmacological activities such as antioxidant, antiparkinsonian, and antidepressant. An analytical method was developed and validated for the estimation of FS by ultrafast liquid chromatography using C-18 reverse phase column. Acetonitrile and orthophosphoric acid (0.2% v/v) in the ratio of 30:70 v/v was used as mobile phase. Flow rate was set at 1 mL/min. Chromatogram of FS was detected at wavelength of 362 nm. Retention time for FS was found to be 7.06 min. The developed method was found to be linear in the range of 2-10 μg/mL with regression coefficient of 0.9985. The method was validated as per the International Conference on Harmonization (ICH) Q2 (R1) guidelines. The percentage recovery was in the range of 95%-105%, which indicated the accuracy of the method. The percentage relative standard deviation (RSD) was found to be <2%, which indicates the precision of the method. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.46 and 1.41 μg/mL, respectively. The developed method was found to be robust as there was no significant change in response with change in flow rate, ratio of mobile phase, and pH. The method was successfully applied for estimation of drug loading and drug release from self-nanoemulsifying drug delivery system (SNEDDS). The % drug loading of FS in prepared liquid SNEDDS formulation was found to be 101.95%. The results of dissolution studies indicated 67.78% FS release in water at the end of 60 min.Based on US EPA detection limit procedure,8 samples with 1-5 times of calculated detection limit were tested.Based on sample standard deviation and student t-distribution,national standard of Aluminum detecting limit was established and verified.Detecting threshold,sample detection limit,and sample quantitative limit were all tested.The method detection Limit is 0.93μg/mL,the reliable quantitative limit is 3.72μg/mL,the sample detection threshold is 93μg/g,the sample quantitative limit is 372μg/g.The sample testing data indicated the testing ability of Aluminum in baking powder.
Sample (material)
Detection threshold
National standard
Cite
Citations (0)
Repeatability
Linearity
Cite
Citations (26)
본 연구에서는 UPLC를 이용한 밀크씨슬추출물의 지표 물질인 실리마린의 신규 분석법을 확립하였으며, 건강기능식품공전의 HPLC 분석법과 비교하여 UPLC 분석법을 검증하였다. UPLC를 이용한 신규 분석법을 검증은 특이성, 직선성, 정확성, 정밀성, 실험실 내 정밀성, 완건성 등 6개의 검증 항목을 선정하여 실시하였다. HPLC 및 UPLC 분석법 모두에서 6가지 실리마린 표준물질이 선택적이며 특이적으로 정확하게 검출됨을 확인하였으며, 실리마린 25-400 μg/mL의 농도에서 결정계수 값이 0.9999이상으로 높은 직선성을 갖음을 확인하였다. 정확성에서 UPLC를 이용한 신규 분석법의 회수율은 평균 99%이상으로 HPLC분석법보다 높은 회수율을 보였으며, UPLC 분석법의 회수율편차가 HPLC 분석의 회수율편차의 절반 이하임을 확인하였다. UPLC 분석법에서 얻어진 피크 면적의 상대표준편차가 HPLC 분석법의 그것과 비교하여 절반 이하였으며, UPLC 분석법의 정밀성 및 실험실 내 정밀성이 HPLC 분석법의 정밀성 및 실험실 내 정밀성보다 높음을 확인하였다. 분석법 검증 결과, 모든 검증 항목에서 HPLC와 UPLC 분석법 모두 적합하게 검증되었으며, 검증 항목 중 정확성, 정밀성, 실험실 내 정밀성 및 완건성 항목에서 UPLC 분석법의 검증값이 HPLC 분석법보다 뛰어났다. HPLC 분석법으로 검체 100개를 분석할 경우, 총 분석시간은 95시간 30분 (기기 안정화 시간 포함한 분석시간은 약 96 시간), 총 이동상 소모량은 6,215 mL이고 이동상 소모량 중 methanol 함량은 2,450 mL이었으나, UPLC 분석법의 총 분석시간은 약 13시간 (기기 안정화 시간 포함한 분석시간은 약 14시간), 총 이동상 소모량은 168 mL이며 이동상 소모량 중 methanol 함량은 74 mL에 불과하였다. 이상의 결과를 통해 UPLC를 이용한 실리마린 신규 분석법은 건강기능식품의 실리마린을 분석하는데 적합하며, 건강기능식품공전의 HPLC 분석법과 비교하여 효율적인 분석법이라고 판단할 수 있다.
Cite
Citations (0)
In non-polluted natural waters, trace metals have generally to be determined near the detection limit of electrothermal atomic absorption spectrometry (ETAAS) and therefore the experimental conditions must be optimized. The detection limit in ETAAS depends strongly on numerous experimental parameters and its optimization is time consuming because, according to IUPAC recommendations, 20 repeated blank measurements per experimental parameter must be performed. In this work, for lead the influence of different experimental parameters on the instrumental detection limit together with the relatively good agreement between experimental and a priori calculated detection limits was demonstrated. The effects of spectroscopic and electrothermal parameters were elucidated from the calculation of detection limits. Under optimized conditions, the detection limit obtained for Pb at 283.3 nm was half that at 217 nm; a 30% improvement was obtained on replacing the hollow-cathode lamp with an electrodeless discharge lamp. The calculation of the detection limit allowed a comparison of atomizers of various geometries and confirmed that high atomization temperatures can be used with the Perkin-Elmer Model 4100ZL spectrometer without degrading the detection limit for Pb. The work on lead also demonstrated that optimizing the integration window by determining the start and end of integration with a computer after smoothing the data significantly improved the detection limit. Under the experimental conditions adopted, using a moving sum of about 20 points led to the lowest detection limit. With a relatively important background absorbance signal, the detection limit for the same dosing volume was improved by using the multiple-injection mode with summation of the resulting atomization signals instead of using the single injection mode.
Absorbance
Cite
Citations (9)
Objective To establish the biologic limit of detection and functional sensitivity of chemiluminescence immunoassay in detection of AFP.Methods Referring to pertinent literature, the RLUs of blank and a serial diluted samples detected by Bayer Centaur 240 chemiluminescense immunoassay system would be calculated to average value, standard deviations and coefficient of variance,which to establish the low limit of detection ,biologic limit of detection and functional sensitivity of AFP.Results The low limit of detection was 1.00 ng/ml and it was lower than the declaration of the manufacturer.The biologic limit of detection was between 2.65 ng/ml and 3.53 ng/ml.The functional sensitivity was 3.53 ng/ml.Conclusion The biologic limit of detection and functional sensitivity must be established in laboratories,which can provide more important information for the clinic.
Chemiluminescent immunoassay
Cite
Citations (0)
Experimental variables in continuous flow hydride generation inductively coupled plasma-optical emission spectrometry (CF-HG-ICP-OES) were optimized for determination of bismuth. Concentrations of NaBH4, HCl, and NaOH, flow rates of NaBH4, sample solution, waste and carrier argon, radio frequency power, lengths of reaction, and stripping coils were optimized to obtain lower detection limits. Under optimum conditions, the detection limit was calculated as 0.16 ng mL−1, and the calibration plot was linear between 1.0–50.0 ng mL−1. An improvement in detection limit of 5.75 times by CF-HG-ICP-OES was reached vs. ICP-OES. Relative standard deviation (RSD) for ten replicate measurements of 10.0 ng mL−1 Bi was calculated as 3.9%. Effect of possible interferic ions on Bi signal was evaluated. Accuracy of method was verified by using a standard reference material, SRM 1643e. Results found for Bi were in satisfactory agreement with certified values. The proposed method was then employed to determine trace concentration of Bi in milk samples. Bi amounts in samples were found in the range from lower than the quantitation limit to 14.5 ng mL−1, whereas Bi concentrations were lower than the detection limit in three samples.
Bismuth
Certified reference materials
Cite
Citations (13)
The feasibility of using a flow injection (FI) hydride generation technique in conjunction with atomic fluorescence spectrometry (AFS) was investigated. Parameters were established for the determination of Sb, As, Bi, Hg, Se and Te. Among the parameters that were found to have a more pronounced influence on performance were the concentration of NaBH4, the carrier gas flow, the observation height and the temperature of the atomizer cell. Compared with the manual sampling system (or batch system), the relative detection limits of the FI combination were better by factors of 2.5–10. By using FI, the sample volume was reduced to 500 mm3, hence, the absolute detection limits were even better with improvements of between 10- and 50-fold depending on the element. The absolute detection limit for Se using the FI technique was 0.035 ng, while with the batch system it was 0.8 ng. Similarly, Hg detection limits with the FI technique and the batch system were found to be 0.015 and 0.4 ng, respectively. The best improvement in the absolute detection limits was found for Te, which with the FI technique was 0.02 ng while with the batch system it was 1.0 ng. The linear ranges were typically 2–3 orders of magnitude of analyte concentrations, which is much wider than that of atomic absorption spectrometry. Sampling frequency was typically 120 injections per hour, and since a double-channel AFS instrument was used in this work, pairs of elements such as As, Sb and Bi, Hg were measured simultaneously, which equates to 240 measurements per hour. The technique was applied to the determination of hydride forming elements in geological reference materials.
Atomic spectroscopy
Cite
Citations (25)
Bacitracin
Chromatographic Separation
Cite
Citations (22)
Linear range
Nanomaterials
Electrochemical gas sensor
Cite
Citations (4)
According to the development of GC equipment, it has been possible to analyze the low level of ambient VOCs concentration. In this study, the limit of detection and the limit of quantitation were estimated for two GC equipments of the VOCs analysis, which would contribute to improve the quality of VOCs analysis results. The results of %RSD for ten standard solutes showed a great reproducibility in terms of detection time and detection area. The limit of detection and the limit of quantitation in SRI GC appeared to be 0.175 ppb and 0.583 ppb for benzene, and 0.223 ppb and 0.743 ppb for toluene, respectively. On the other hand, The limit of detection and the limit of quantitation in FISON GC appeared to be 0.149 ppb and 0.496 ppb for benzene, and 0.094 ppb and 0.313 ppb for toluene, respectively.
Cite
Citations (0)