scholarly journals VERIFIKASI METODE ANALISIS METAMFETAMINA DAN AMFETAMINA DALAM MATRIKS URIN SECARA AUTOMATISASI DENGAN GERSTEL® DISPOSABLE PIPETTE EXTRACTION (DPX) MULTIPURPOSE SAMPLER (MPS)

2021 ◽  
Vol 1 (3) ◽  
pp. 31-38
Author(s):  
Prisma Andini Mukti ◽  
Sulaeman Mappasessu ◽  
Yuswardi Mappasessu ◽  
Triwidiastuti Andini Mukti ◽  
Dwi Hernanto ◽  
...  

Method analytical validation and verification is crucial in routine qualitative and quantitative analysis. Analysis laboratory need objective evidences about specific parameters in their drugs/analytes or drugs metabolites in matrices biology. Urine is the most preferable matrix biology for determining drugs metabolites especially in drug abuses cases because urine’s sampling process is not invasive. There are many methods extracting drugs in urine, especially methamphetamine and amphetamine as those two analytes are excreted via urine. This study presented method verification for determination of methamphetamine and amphetamine in urine using Gerstel® automated Disposable Pipette Extraction (DPX) Multipurpose Sampler (MPS). Result of this study showed that retention time of methamphetamine is in minute 6.21, and amphetamine is in minute 3.15. Methampethamine’s curve displayed a coefficient of determination r2=0,9999 with the equation y=170,19x+33183. The equation of amphetamine showed y=44390x – 17513 with coefficient of determination r2= 0,9974. Limit of detection (LOD) of methamphetamine in urine is 59,73 ppb, and LOD of amphetamine is 36 ppb.

Molecules ◽  
2021 ◽  
Vol 26 (6) ◽  
pp. 1602
Author(s):  
Ya-Ping Guo ◽  
Hong Yang ◽  
Ya-Li Wang ◽  
Xiao-Xiang Chen ◽  
Ke Zhang ◽  
...  

Crataegi folium have been used as medicinal and food materials worldwide due to its pharmacological activities. Although the leaves of Crataegus songorica (CS), Crataegus altaica (CA) and Crataegus kansuensis (CK) have rich resources in Xinjiang, China, they can not provide insights into edible and medicinal aspects. Few reports are available on the qualitative and quantitative analysis of flavonoids compounds of their leaves. Therefore, it is necessary to develop efficient methods to determine qualitative and quantitative flavonoids compounds in leaves of CS, CA and CK. In the study, 28 unique compounds were identified in CS versus CK by qualitative analysis. The validated quantitative method was employed to determine the content of eight flavonoids of the leaves of CS, CA and CK within 6 min. The total content of eight flavonoids was 7.8–15.1 mg/g, 0.1–9.1 mg/g and 4.8–10.7 mg/g in the leaves of CS, CA and CK respectively. Besides, the best harvesting periods of the three species were from 17th to 26th September for CS, from 30th September to 15th October for CA and CK. The validated and time-saving method was successfully implemented for the analysis of the content of eight flavonoids compounds in CS, CA and CK for the first time.


2021 ◽  
Author(s):  
Yiwen Cao ◽  
Shenjie Zhu ◽  
Lin Zhang ◽  
Qun Cui ◽  
Haiyan Wang

Aiming at the difficulty in qualitative and quantitative analysis of trace compositions in food preservative propionic acid, the trace compositions and the key components influencing the total aldehyde content in...


2012 ◽  
Vol 468-471 ◽  
pp. 1104-1109
Author(s):  
Hui Ying Yu ◽  
Ping Yan

Adopting raman spectrometer to conduct qualitative and quantitative analysis of m-cresol and p-cresol, selecting the respective character peak of bencycloquidium after deformation vibration (m-cresol at 732 cm-1 and p-cresol at 841 cm-1), via experiment and calculations, the relative raman cross section of m-cresol and p-cresol can be concluded:(∂σ/∂Ω)732cm-1/(∂σ/∂Ω)1000cm-1 is 0.74 (height-fitting of the peak), and 0.61 (area-fitting of the peak). This method samples simply and rapidly, and has a short testing time, whose quantitative analysis result of m-/p-cresol is consistent with that of GC analysis.


2021 ◽  
Vol 10 (1) ◽  
pp. 20-28
Author(s):  
Ivana Savić-Gajić ◽  
Ivan Savić ◽  
Predrag Sibinović ◽  
Valentina Marinković

In this study, the modified stability-indicating RP-HPLC method was validated for quantitative analysis of amlodipine besylate in the presence of its impurity D (3-ethyl 5-methyl 2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-6-methylpyridine-3,5-dicarboxylate). The method was applied for the determination of an analyte in the tablets and irradiated samples packed in the primary packaging (Alu/PVC/PVDC blister packaging). The efficient chromatographic separation was achieved using a ZORBAX Eclipse XDB-C18 column (4.6×250 mm, 5 mm) with isocratic elution of mobile phase which consisted of acetonitrile:methanol:triethylamine solution (15:35:50, v/v/v) (pH 3.0). The flow rate of the mobile phase was 1 mL min-1, while the detection of amlodipine besylate was carried out at 273 nm. Amlodipine besylate and its impurity D were identified at the retention times of 16.529 min and 2.575 min, respectively. The linearity of the method with the coefficient of determination of 0.999 was confirmed in the concentration range of 10 - 75 µg mL-1 for amlodipine besylate. The limit of detection was 0.2 µg mL-1, while the limit of quantification was 0.66 µg mL-1. After UV and Vis radiation of the tablets packed in the primary packaging, the content of amlodipine besylate was reduced by 22.38% and 19.89%, respectively. The presence of new degradation products was not detected under the given chromatographic conditions. The photodegradation of amlodipine besylate followed pseudo-first-order kinetics. Based on the half-life of amlodipine besylate (38.4 days for UV radiation and 43.3 days for Vis radiation), it was concluded that amlodipine besylate in the tablets has satisfactory photostability after its packing in the Alu/PVC/PVDC blister packaging.


Molecules ◽  
2018 ◽  
Vol 23 (7) ◽  
pp. 1813 ◽  
Author(s):  
Özlem Bahadır-Acıkara ◽  
Serkan Özbilgin ◽  
Gülcin Saltan-İşcan ◽  
Stefano Dall’Acqua ◽  
Veronika Rjašková ◽  
...  

Previously tested n-hexane extracts of the Scorzonera latifolia showed promising bioactivity in vivo. Because triterpenes could account for this activity, n-hexane extracts were analyzed by HPLC to identify and quantify the triterpenes as the most abundant constituents. Other Scorzonera and Podospermum species, potentially containing triterpenic aglycones, were included in the study. An HPLC method for simultaneous determination of triterpene aglycones was therefore developed for analysis of Podospermum and Scorzonera species. n-Hexane extracts of root and aerial parts of S. latifolia, ten other Scorzonera species and two Podospermum species were studied to compare the content of triterpenes. HPLC was used for the qualitative and quantitative analysis of α-amyrin, lupeol, lupeol acetate, taraxasteryl acetate, 3-β-hydroxy-fern-7-en-6-one acetate, urs-12-en-11-one-3-acetyl, 3-β-hydroxy-fern-8-en-7-one acetate, and olean-12-en-11-one-3-acetyl. Limits of detection and quantification were determined for each compound. HPLC fingerprinting of n-hexane extracts of Podospermum and Scorzonera species revealed relatively large amounts of triterpenes in a majority of investigated taxa. Lupeol, lupeol acetate, and taraxasteryl acetate were found in a majority of the species, except S. acuminata. The presence of α-amyrin, 3β-hydroxy-fern-7-en-6-one-acetate, urs-12-en-11-one-3-acetyl, 3β-hydroxy-fern-8-en-7-one-acetate, and olean-12-en-11-one-3-acetyl was detected in varying amounts. The triterpene content could correlate with the analgesic and anti-inflammatory activity of Scorzonera, which was previously observed and Scorzonera species that have been determined to contain triterpenes in large amounts and have not yet been tested for their analgesic activity should be tested for their potential analgesic and anti-inflammatory potential. The presented HPLC method can be used for analysis of triterpene aglycones, for example dedicated to chemosystematic studies of the Scorzonerinae.


1964 ◽  
Vol 8 ◽  
pp. 456-461
Author(s):  
Donald Mitcham ◽  
Biagio Piccolo ◽  
Verne W. Tripp ◽  
Robert T. O’Connor

AbstractThe application of X-ray fluorescence to the qualitative and quantitative analysis of chemically modified cotton textile materials is described. The scope and flexibility of the technique have permitted the determination of more than 20 elements with, greatly reduced elapsed time compared with the corresponding spectroscopic or wet methods. Precautions to be observed in preparing standards are discussed. Results of the analysis of typical modifications and their significance in the development of cottons for specific uses are described.


2019 ◽  
Vol 2019 ◽  
pp. 1-8
Author(s):  
Mohammad F. Hossain ◽  
Mamoon Rashid ◽  
Rajjit Sidhu ◽  
Randy Mullins ◽  
Susan L. Mayhew

Mushrooms have been used as part of the average diet and as a nutraceutical for thousands of years due to their immense health benefits. The purpose of this study was to develop a simple, fast, accurate, specific, reproducible, and robust chromatographic method to identify and quantify two water-soluble vitamins: thiamine (B1) and riboflavin (B2) in mushrooms. The method employed for qualitative and quantitative analysis of these vitamins was Reversed Phase-High Performance Liquid Chromatography (RP-HPLC) equipped with Ultraviolet–Visible (UV-Vis) Detector. The extraction process involved acid hydrolysis followed by enzymatic dephosphorylation with takadiastase enzyme. Chromatographic separation was achieved with a Shimadzu prominence HPLC system using isocratic elution mode on a Waters Xterra® MS C-18 column (4.6mm × 150mm, 5 μm) integrated with a XBridge® BEH C-18 Guard column (2.1mm × 5 mm, 5 μm). The mobile phase of this study consisted of buffer and methanol in the ratio of 80:20, where the buffer contained sodium-1-hexanesulfonate, glacial acetic acid, methanol, and pH adjusted to 3.0 with diethylamine. Vitamins were detected simultaneously at their lambda max wavelengths B1: 245nm and B2: 268nm using dual-wavelength UV detection technique to get their highest response. The proposed method was found to be specific, linear R>1.0, accurate, precise (% recovery ± SD; B1:104.45±4.5 and B2: 104.88±2.04), sensitive, (limit of detection for B1 and B2 was 0.043 and 0.029 μg/mL, respectively), and robust for mushrooms analysis. No coeluting peaks were observed at the retention time of the vitamins and all the peaks were spectrally homogenous. The standard and sample solutions were found to remain stable at cold temperature for 72 hours. In summary, our data suggest that the proposed method could be used in food industries to monitor the product quality during routine quality control purposes.


1982 ◽  
Vol 65 (3) ◽  
pp. 745-752
Author(s):  
U D O Pechanek ◽  
Gernot Blaicher ◽  
Werner Pfannhauser ◽  
Herbert Woidich

Abstract An electrophoretic method has been developed for qualitative and quantitative determination of all common thickening and gelling agents. Thickeners were identified by their migration behavior, their staining ability, and the characteristic shapes of their electrophoretic zones, and then quantitated in a scanner. A method is also reported for isolating thickeners from food, including removal of fat and dyes by dioxane, enzymatic starch degradation, removal of protein by trichloroacetic acid, and precipitation of the polysaccharides by absolute ethanol. Isolation of gelatin is also described.


2016 ◽  
Vol 2016 ◽  
pp. 1-9 ◽  
Author(s):  
Chukwuma S. Ezeonu ◽  
Chigozie M. Ejikeme

The phytochemical contents of some milled Nigerian softwood chips were carried out in a quest to evaluate their potentials as sources of alternative medicine as well as uses in other industrial applications. The qualitative and quantitative analysis were ascertained. Tannin was found in all the Nigerian softwoods examined with the highest quantities obtained in Sterculia oblonga (1240 mg/100 g) and Barteria nigritiana (1230 mg/100 g). Highest quantities of alkaloid were obtained in Cordia millenii (11.2%) and Sterculia oblonga (10.4%). Barteria nigritiana (14.2%) and Moringa oleifera (12.2%) recorded more flavonoid content than other individual softwoods. Saponin was more in Anogeissus leiocarpus (12.5%) and Dichrostachys cinerea (9.8%). Oxalate was found to be higher in Combretodendron macrocarpum (5.84 g/100 g) and Glyphaea brevis (3.55 g/100 g). Pentaclethra macrophylla (890 mg/100 g) and Moringa oleifera (880 mg/100 g) contained more cyanogenic glycosides. Sacoglottis gabonensis (4.68 mg/g) and Pentaclethra macrophylla (4.04 mg/g) showed the highest contents of phenol, while more lipids (8% and 7.2%) were found in Anogeissus leiocarpus and Kaempferia galanga, respectively. The results showed that these Nigerian softwoods grains could be a source for the exploitation of these phytochemicals beneficial in the pharmaceutical and alternative medicine industries.


2018 ◽  
Vol 101 (3) ◽  
pp. 708-713
Author(s):  
Anna Maślanka ◽  
Mariusz Stolarczyk ◽  
Anna Apola ◽  
Anna Kwiecień ◽  
Urszula Hubicka ◽  
...  

Abstract A new chromatographic-densitometric method has been developed for the qualitative and quantitative determination of the active ingredients in a simulated mixture corresponding to the PolyIran polypill, composed of acetylsalicylic acid, hydrochlorothiazide (HCT), enalapril (ENA), and atorvastatin (ATR), whose efficacy in the treatment and prevention of cardiovascular disease has been documented in clinical trials. Chromatographic separation was performed using TLC silica gel 60 plates with fluorescent indicator F254 as the stationary phase and a mixture of n-hexane–ethyl acetate–methanol–water–acetic acid (8.4 + 8 + 3 + 0.4 + 0.2, v/v/v/v/v) as the mobile phase. Densitometric measurements were carried out at λ = 210 nm when determining ENA and at λ = 265 nm in the case of the other drugs. Peaks of examined substances were well separated in the recorded chromatograms, enabling the evaluation of the results in terms of both qualitative and quantitative analysis. The method was specific for the analyzed components and was characterized by high sensitivity. The LOD was between 0.043 and 0.331 μg/spot, and LOQ was between 0.100 and 0.942 μg/spot. Recovery was in the range of 97.02–101.34%. The linearity range was broad and ranged from 0.600 to 6.000 μg/spot for acetylsalicylic acid, from 0.058 to 1.102 μg/spot for HCT, from 0.505 to 6.560 μg/spot for ENA, and from 0.100 to 1.000 μg/spot for ATR. The method was characterized by good precision, with RSD values that ranged from 0.10 to 2.26%.


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