scholarly journals Validation of Method for Determining Alpha- Mangostin Level of Ethyl Acetate Extract of Mangosteen Rind Using TLCSpectrodensitometry

2017 ◽  
Vol 1 (1) ◽  
pp. 1
Author(s):  
N. P. A. D. Wijayanti ◽  
L.P.M.K. Dewi ◽  
K.W. Astuti
Keyword(s):  
Ethyl Acetate ◽  
Analytical Method ◽  
Ethyl Acetate Extract ◽  
Limit Of Detection ◽  
Maximum Amount ◽  
Garcinia Mangostana ◽  
Percent Recovery ◽  
Limit Of Quantitation ◽  
Aging Properties ◽  
Spectrum Correlation

Abstract Objective: Mangosteen rind (Garcinia mangostana L.) contains secondary metabolites, namely alpha-mangostin which has antioxidant activity, as well as antibacterial and anti-aging properties. In order to obtain a maximum amount of alpha-mangostin compounds, the maceration method using ethyl acetate was used. To ensure the effectiveness of the mangosteen rind extraction process, all of the processes and methods in preparing the extract should be properly controlled, particularly the analytical method used in determining the alpha-mangostin level of the extract. The method used should be able to determine the alphamangosteen level accurately. This study aimed to test the validation of the analytical method used. Method: The parameters for the validation of the analytical method tested in this study include accuracy, precision, range and linearity, limit of detection (LOD), limit of quantitation (LOQ) and specificity. In this study, the level of alpha-mangostin in the extract was determined using TLC-Spectrodensitometry with the stationary phase of the silica gel plate GF 254 and the mobile phase of chloroform and methanol (10:0.1 v/v). Result: The results of the study showed that this method has met the acceptance criteria for validation with the accuracy value in the range of percent recovery, from 93.85 % to 111.16%; precision with KV <2%; specification with spectrum correlation >0.99; linearity with r =0,99372; limit of detection (LOD) of 5.33 ng and limit of quantitation (LOQ) of 11.43 ng.

P–006 Simultaneous determination of bisphenol A and S in the samples of human seminal fluid

2021 ◽  
Vol 36 (Supplement_1) ◽  
Author(s):  
S Fialková ◽  
T Král ◽  
J Kohoutek ◽  
K Franzová ◽  
M Ješeta ◽  
...  
Keyword(s):  
Sample Preparation ◽  
Bisphenol A ◽  
Endocrine Disruptors ◽  
Analytical Method ◽  
Seminal Fluid ◽  
Limit Of Detection ◽  
Semen Parameters ◽  
Ms Detection ◽  
Validation Criteria ◽  
Limit Of Quantitation

Abstract Study question Can we quantitatively determine concentrations of endocrine disruptors namely bisphenol A and S in seminal fluid? Summary answer We developed selective analytical method to simultaneously screen for the presence of bisphenol A (BPA) and S (BPS). What is known already The male reproductive system involves processes, which may be influenced by the disruption of the endocrine system by chemicals called endocrine disruptors (EDs). There is a growing evidence that EDs such as bisphenol A and S may be responsible for the decline in male reproductive health. To date, the claimed adverse effects on male fertility are largely based on the results from studies assessing the relationship between urinary BPA and BPS concentration and semen parameters. The best evidence of an adverse effect of BPA and BPS directly on spermatozoa could be provided by measuring bisphenols concentration directly in seminal fluid. Study design, size, duration To selectively and quantitatively analyzed bisphenols in any biological matrix advanced analytical tools and selective sample preparation protocols must be employed. In this study we developed targeted analytical method based on liquid chromatography tandem mass (LC-MS/MS) detection to measure bisphenol A and S in seminal fluid samples obtained from IVF clinic. A total of 140 samples were analysed. Participants/materials, setting, methods BPA and BPS was extracted from 140 seminal fluid samples using solvent extraction followed by preconcentration step. Samples were analyzed on Agilent 6495 Triple Quadrupole (Agilent Technologies, Santa Clara, CA) operating in the ESI-negative mode. Two MS/MS transitions were used for quantitative LC-MS/MS analyses. Chromatographic separation was achieved on Waters™ ACQUITY™ UPLC™BEH C18 (100 × 2.1 mm, 1.7 µm) column using gradient elution with a mixture of 0.1mM ammonium fluoride and methanol as mobile phases. Main results and the role of chance We developed selective sample preparation method for detection of BPA and BPS in seminal fluid followed by LC-MS/MS detection. The method validation was performed based on FDA guidelines. Validation criteria included limit of detection (LOD), limit of quantitation (LOQ), accuracy and precision. Due to the lack of the certified reference material the validation criteria of the method were assessed in pool of spiked seminal samples. The accuracy of the LC-MS/MS method was evaluated as a percent recovery of the amount of target analyte added into the sample. Recovery rates were above 80% for both analytes. LOD was 0.04 ng/mL for BPA and 0.01 ng/mL for BPS. LOQ was 0.14 ng/mL and 0.02 ng/mL for BPS. Measured BPA concentration ranged from 0.04 ng/mL to 1.62 ng/mL. For BPS, the concentration ranged from 0.01 ng/mL to 0.47 ng/mL. BPA and BPS were detected in 64% and 81% of samples, respectively. Interestingly, BPA showed lower detection frequency compared to BPS. These results are consistent with other studies performed on urine samples. Limitations, reasons for caution The limitation of the developed method is the time-consuming sample preparation and analysis cost. Wider implications of the findings: These results document for the first time the presence of BPS in seminal fluid. Knowing the concentration of BPA and BPS in seminal fluid is crucial for mitigating the associated health risks and initiating intervention and prevention strategies. Our future work will evaluate the influence of BPS concentration on spermatozoa. Trial registration number AZV NV18–01–00544; CZ.02.2.69/0.0/0.0/19_074/0012727

scholarly journals THE RAPID AND GREEN HAIR ANALYSIS METHOD DEVELOPMENT USING FTIR FOR PAPAVERINE HCL DETERMINATION

2019 ◽  
pp. 211-217 ◽  
Author(s):  
ILMA NUGRAHANI ◽  
STEPHANIE SULISTIANA ◽  
SLAMET IBRAHIM
Keyword(s):  
Hair Sample ◽  
Method Development ◽  
Limit Of Detection ◽  
Area Under The Curve ◽  
Forensic Analysis ◽  
Percent Recovery ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Papaverine Hydrochloride

Objective: This study was aimed to develop a rapid analysis using FTIR (Fourier Transform Infra-Red) for papaverine hydrochloride (HCl) determination in the hair sample, supported by a mathematically manipulation; which never been reported before in toxicology and forensic analysis. Methods: Firstly, the method was checked its validity to ensure the feasibility for the quantitative purpose. The absorbance spectrums were collected by measure the drug, matrix, and its mixture. A spectra which showed the best specificity and linearity then was selected and derived. Afterwards, the area under the curve (AUC) was measured. A series of concentration was used for compose the calibration curve. Based on the result, some validation parameters were checked thoroughly. Further, for sample preparation, hair was collected non-invasively, then was decontaminated using soap. Next, it was immersed into a papaverine HCl solution at a concentration of 25 mg/ml along days. Finally, the amount of drugs absorbed were measured by the developed method using FTIR. Results: Experimental data showed that all validation parameters could be fulfilled by the developed method. The selected spectra for the content determination was 1320-1230 cm-1. Its linearity was represented by a correlation coefficient value (r) ≥ 0.9999, variation coefficient (Vxo) ≤ 2.0%. The limit of detection (LOD) was 0.00618% w/w, meanwhile, the limit of quantitation (LOQ) was 0.02060% w/w, respectively. The percent recovery was in the range 97-103% with the relative standard deviation (RSD) was ≤ 2.0%. The drug has detected after 72 h immersion, moreover, after 192 h the concentration gained was 0.1594±0.0011% w/w. Conclusion: As the conclusion, FTIR absorbance-derivative method is adequate as a rapid procedure for determine papaverine HCl in the hair sample. This method shows the appropriate of specificity, accuracy and precise. In addition, it shows the advantages of simplicity, green/eco-friendlier, and cost-efficiency.

scholarly journals DEVELOPMENT OF A DIRECT METHOD OF ANALYZING TRANEXAMIC ACID LEVELS IN WHITENING CREAM USING REVERSED PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2020 ◽  
pp. 88-92
Author(s):  
BAITHA PALANGGATAN MAGGADANI ◽  
JIHAN YASMINA ◽  
HARMITA HARMITA
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Tranexamic Acid ◽  
Analytical Method ◽  
High Performance ◽  
Limit Of Detection ◽  
Direct Method ◽  
Pharmaceutical Products ◽  
Optimal Method ◽  
Limit Of Quantitation

Objective: Whitening cream is a cosmetic that contains ingredients that can alleviate hyperpigmentation. Tranexamic acid (TA) is one of the potentialanti-pigmentation agents that work through inhibiting plasmin. TA is used in cosmetic formulations at a concentration of 2.5% as a whitening andmoisturizing agent. To date, research on TA in both cosmetics and other pharmaceutical products using high-performance liquid chromatography(HPLC) has not been done directly (without derivatization). Therefore, this study aimed to develop a simple and rapid analytical method for TA(without derivatization) in cosmetic cream samples using reverse-phase HPLC and water as a solvent.Methods: Optimization was conducted by evaluating several parameters that affect sample extraction, as well as composition and mobile phasetypes. The optimal method must fulfill suitability and validation requirements. The optimal method should be able to detect and quantify TA in creamsamples without derivatization.Results: The optimal analysis condition used a ultraviolet detector at a wavelength of 210 nm, acetonitrile: double-distilled water: phosphoric acid(64:34:2) as the mobile phase and a flow rate of 0.8 mL/min. The retention time of the analyte occurred in the 2nd min.Conclusion: The analytical method that met the validation requirements was characterized using parameters such as accuracy, precision, linearity,selectivity, limit, of detection, and limit of quantitation. This method is applicable for analyzing TA content in samples with a concentration of 1.02%.

Development and validation of a HPLC-UV method for the simultaneous detection and quantification of paclitaxel and sulforaphane in lipid based self-microemulsifying formulation

2019 ◽  
Vol 57 (10) ◽  
pp. 931-938 ◽  
Author(s):  
Mohammad M Kamal ◽  
Sami Nazzal
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Simultaneous Detection ◽  
Reversed Phase ◽  
Limit Of Quantitation ◽  
Development And Validation ◽  
Simultaneous Delivery ◽  
Detection And Quantification

Abstract Paclitaxel (PTX) and sulforaphane (SFN) are known anticancer molecules. Their activity was found to be potentiated when tested concurrently. Only recently, however, a novel SFN enabled PTX self-microemulsifying formulation (SMEDDS) was developed for their simultaneous delivery. This necessitated the development of an analytical method for the simultaneous detection and quantitation of PTX and SFN. In this study, a simple and sensitive isocratic high performance liquid chromatography-ultraviolet (HPLC-UV) analytical method was developed and validated per International Conference on Harmonization guidelines to satisfy this objective. Its application was demonstrated when quantifying the amount of PTX and SFN released from the SMEDDS in various dissolution media. The separation of the analytes was performed with the aid of a reversed phase C18 column at ambient temperature using a 60:40 mixture of acetonitrile and KH2PO4 buffer (pH 5.0) as the mobile phase. PTX and SFN peaks were detected at 202 nm with high resolution without interference from excipients. This method showed linearity within 2.5–100 μg/mL range with r2 &gt; 0.999. The limit of detection and lower limit of quantitation were 0.1638 and 0.4964 μg/mL for PTX and 0.4419 and 1.3389 μg/mL for SFN, respectively. A total of 98–101% of the injected samples was recovered with RSD of 0.06–0.68% indicating the suitability of the method for the simultaneous detection and quantitation of the molecules in dissolution media.

scholarly journals The presence of endophytic actinobacteria in mangosteen peel (Garcinia mangostana) and its antioxidant activity

2020 ◽  
Vol 21 (4) ◽  
Author(s):  
Fily Larasati ◽  
IRMANIDA BATUBARA ◽  
YULIN LESTARI
Keyword(s):  
Antioxidant Activity ◽  
Ethyl Acetate ◽  
Antioxidant Capacity ◽  
Ethyl Acetate Extract ◽  
Antioxidant Properties ◽  
Rrna Gene ◽  
Blue Color ◽  
Garcinia Mangostana ◽  
Mangosteen Peel ◽  
Endophytic Actinobacteria

Abstract. Larasati F, Batubara I, Lestari Y. 2020. The presence of endophytic actinobacteria in mangosteen peel (Garcinia mangostana L.) and its antioxidant activity. Biodiversitas 21: 1488-1497. Mangosteen (Garcinia mangostana L.) is a family member of Clusiaceae which is rich in secondary metabolite compounds that can function as antioxidants. Besides being produced by its host plant, the bioactive compounds can also be produced by endophytic actinobacteria. The purpose of this study was to explore the presence of endophytic actinobacteria from mangosteen peel and determine its antioxidant activity. The actinobacteria were isolated, purified, morphologically characterized, molecularly identified, extracted with ethyl acetate and tested for antioxidant properties. The antioxidant activity was assayed using DPPH (2.2-diphenyl-1-picrylhydrazyl) and ABTS (2,2′-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) methods. The components of extracts were separated by Thin Layer Chromatography (TLC) and bioautography was done to determine the antioxidant bands. As a result, five isolates of endophytic actinobacteria in mangosteen peel showed to have difference in aerial mycelium color, substrate mycelium color, and types of spore chains. Based on 16S rRNA gene analysis, AGM3.2 isolate showed similarity with Streptomyces griseochromogenes ATCC 14511 (T) 99.06%. AGM3.1 had similarity with Streptomyces osmaniensis OU-63 (T) 98.35%. Meanwhile, AGM2.3 were similar to Streptomyces xanthophaeus NBRC B-5414 (T) 99.82%, AGM2.2 had similarity with Streptomyces xanthophaeus NBRC B-5414 (T) 98.95%. In addition, AGM2.1 has homology with Streptomyces goshikiensis NBRC 12868 (T) 99.52%. Using both DPPH and ABTS, supernatant of AGM2.1 showed the highest antioxidant activity indicated by 36.96 and 98.80 inhibition, respectively. Antioxidant capacity of ethyl acetate extract of AGM2.1 was 22.22 μg AEAC/mg extract (DPPH) and 20.34 μg AEAC/mg extract (ABTS). Meanwhile, ethyl acetate extract of mangosteen peel had antioxidant capacity by 21.17 µg AEAC/mg extract (DPPH) and 18.75 µg AEAC/mg extract (ABTS). Antioxidant bioautographic analysis of mangosteen peel ethyl acetate extract was compared with alpha mangosteen standard. The results showed that alpha mangosteen presence in the mangosteen extract with the same Rf value of 0.64 with standard. Meanwhile, actinobacterial ethyl acetate extract from AGM3.1, AGM2.3, AGM2.2, AGM2.1 each have the same Rf value with the alpha mangosteen standard. However, the spot for alpha mangosteen had dark red color, while spots of the four actinobacterial isolates showed to have blue color indicating different antioxidant compounds. The blue spot indicates the flavone, flavanone, flavonol, and isoflavone. These compounds include a subgroup of flavonoid compounds. Ethyl acetate extract AGM3.2 does not have spot compounds with the same Rf value as the alpha mangosteen standard. Study clearly shows that endophytic actinobacteria from mangosteen peel have potency as antioxidant.

scholarly journals ANTIBAKTERI EKSTRAK KULIT BUAH MANGGIS (Garcinia mangostana L.)

2017 ◽  
Vol 4 (2) ◽  
pp. 172
Author(s):  
Srikandi Srikandi ◽  
I.G.A. Manik Widhyastini
Keyword(s):  
Staphylococcus Aureus ◽  
Pseudomonas Aeruginosa ◽  
Ethyl Acetate ◽  
Inhibitory Concentration ◽  
Ethyl Acetate Extract ◽  
Inhibition Zone ◽  
Solvent Concentration ◽  
Garcinia Mangostana ◽  
A Value ◽  
Hexane Extracts

Antibacterial Extract of Mangosteen (Garcinia mangostana L.)Fruit Shell           The skin of the mangosteen fruit is extracted with n-hexane and ethyl acetate to determine the Minimum Inhibitory Concentration (MIC) against Staphylococcus aureus ATCC 25923 and Pseudomonas aeruginosa ATCC 27 853. Results showed that n-hexane extract gave inhibition zone larger than the ethyl acetate extract on all concentrations . Extract n-hexane has a value of MIC against S. aureus ATCC bacterial test 25923 62.5 mg / ml while the ethyl acetate extract of 125 mg / ml . N- hexane extracts had MIC values of the test bacteria P.aeuroginosa ATCC 27 853 was 125 mg / ml , and while the ethyl acetate extract had a MIC value of 500 mg / ml . Treatment of solvent, concentration and interaction between the solvent and concentration significantly affected the test bacteria ATCC 25923 S. aureus at the level of 5 %, the highest interaction N-Hexane solvent with a concentration of 15,625 mg / ml and was not significantly different interactions with the concentration of 31.25 mg/ml and 125 mg/ml. Treatment solvent and concentration significantly while the interaction between the solvent and the concentration has no effect on the test bacteria P.aeuroginosa ATCC 27 853 at 5% level .Keywords: Garcinia mangostana L., Staphylococcus aureus and Pseudomonas aeruginosa ABSTRAK           Kulit buah manggis diekstrak dengan n-heksan dan etil asetat   untuk mengetahui Konsentrasi Hambat Minimum (KHTM) terhadap bakteri Staphylococcus aureus ATCC 25923 dan Pseudomonas aeruginosa ATCC 27853. Hasil penelitian menunjukkan bahwa ekstrak n-heksana  memberikan zona hambatan lebih besar dibandingkan dengan ekstrak etil asetat pada semua konsentrasi. Ekstrak n-heksana  memiliki nilai kadar hambat minimal (KHM) terhadap bakteri uji S. aureus ATCC 25923  62,5 mg/ml sedangkan ekstrak etil asetat 125 mg/ml.   Ekstrak n-heksana memiliki nilai KHM   terhadap bakteri uji P.aeuroginosa  ATCC 27853 adalah 125 mg/ml dan  sedangkan ekstrak etil asetat memiliki nilai KHM  500 mg/ml. Perlakuan pelarut, konsentrasi dan interaksi antara pelarut dan konsentrasi  berpengaruh nyata terhadap bakteri uji S. aureus ATCC 25923 pada taraf 5%, interaksi tertinggi yaitu pelarut N-Heksan dengan konsentrasi 15,625mg/ml dan interaksi ini tidak berbeda nyata dengan konsentrasi 31,25 mg/ml dan 125 mg/ml. Perlakuan pelarut dan konsentrasi  berpengaruh nyata sedangkan interaksi antara pelarut dan konsentrasi  tidak berpengaruh terhadap bakteri uji P.aeuroginosa  ATCC 27853 pada taraf 5%. Kata kunci:  Garcinia mangostana L., Staphylococcus aureus dan Pseudomonas aeruginosa

scholarly journals HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY ANALYTICAL METHOD VALIDATION FOR GLUTARALDEHYDE AND BENZALKONIUM CHLORIDE IN DISINFECTANTS

2018 ◽  
Vol 10 (1) ◽  
pp. 248
Author(s):  
Baitha Palanggatan Maggadani ◽  
Harmita . ◽  
Maizura Isfadhila
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Analytical Method ◽  
Benzalkonium Chloride ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Analytical Method Validation ◽  
Limit Of Quantitation ◽  
Uv Visible

Objective: The aim of this study was to produce a selective, accurate, and faster high-performance liquid chromatography (HPLC) analytical methodfor benzalkonium chloride and glutaraldehyde in disinfectants using ultraviolet (UV)-visible detection.Methods: Glutaraldehyde has no chromophore, so it was first derivatized using 2,4 dinitro phenylhydrazine. Acetonitrile:water (75:25) was used asthe mobile phase for glutaraldehyde and acetonitrile-acetate pH 4 (75:25) for benzalkonium chloride, both at a flow rate of 1.2 mL/min. The optimizedassay was validated with respect to accuracy, precision, linearity, selectivity, limit of quantitation (LOQ), and limit of detection (LOD).Results: The method was linear for benzalkonium chloride, with correlation coefficient of 0.9995, LOD of 14.55 ppm, and LOQ of 48.51 ppm. Thecorrelation coefficient for glutaraldehyde was 0.9995, with LOD of 0.49 ppm and LOQ of 1.64 ppm. Accuracy was between 98% and 102%, andprecision was below 2% for both the tests.Conclusion: The HPLC analytical method for benzalkonium chloride and glutaraldehyde in disinfectants using UV-visible detection in this researchwas successful to produce a selective, accurate, and faster method.

scholarly journals Development and Validation of a Spectrophotometric Method for Quantification and Dissolution Studies of Glimepiride in Tablets

2012 ◽  
Vol 9 (2) ◽  
pp. 993-998
Author(s):  
Madhusudhanareddy Induri ◽  
Bhagavan Raju M. ◽  
Rajendra Prasad Y. ◽  
Pavankumar Reddy K.
Keyword(s):  
Quantitative Determination ◽  
Spectrophotometric Method ◽  
Analytical Method ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Spectrophotometric Methods ◽  
Dissolution Studies ◽  
Limit Of Quantitation ◽  
Development And Validation

The objective of present study was to develop and validate an analytical method for quantitative determination and dissolution studies of glimepiride in tablets. The glimepiride shows absorption maxima at 225 nm and obeyed Beer's law in the range of 6.0 – 14.0 µg/mL. The limit of detection and limit of quantitation were 0.06, and 0.17 µg/mL respectively. Percentage recovery of glimepiride for the proposed method ranged from 99.32 to 100.98% indicating no interference of the tablet excipients. It was concluded that the proposed method is simple, easy to apply, economical and used as an alternative to the existing spectrophotometric and non-spectrophotometric methods for the routine analysis of glimepiride in pharmaceutical formulations andin vitrodissolution studies.

scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR ANALYSIS OF DEOXYARBUTININ ANHYDROUS EMULSION SYSTEM USING HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2019 ◽  
pp. 172-175 ◽  
Author(s):  
MUCHTARIDI MUCHTARIDI ◽  
IDA MUSFIROH ◽  
AHMAD FAUZI
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Analytical Method ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Emulsion System ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: The aim of this study is to develop a simple, precise and accurate analytical method of deoxyarbutin in anhydrous emulsion system preparation. Methods: The analysis was conducted using high-performance liquid chromatography (HPLC). Chromatographic analysis was carried out using a reversed phase-C18 column. The mobile consists of two phases methanol and water (60: 40 v/v) at a flow rate of 1.0 ml/min. The determinations were performed using UV detector set at 225 nm. All validation procedures were added with hydroquinone as an internal standard. Results: The method showed coefficient correlation is 0.9978, relative standard deviation (RSD) smaller than 2%, Limit of Detection (LOD) and Limit of Quantitation (LOQ) are 0.599 µg/ml and 1.817 µg/ml respectively. The total amount deoxyarbutin in anhydrous emulsion preparation is 1.964+0.02 % with 98% recovery percentage. Conclusion: The developed HPLC analytical method meets the validation criteria made by International Conference on Harmonisation (ICH).

scholarly journals Determination of residual solvents in paclitaxel by headspace gas chromatography

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Khaleel Noorbasha ◽  
Abdul Rahaman Shaik
Keyword(s):  
Ethyl Acetate ◽  
Chromatographic Method ◽  
Isopropyl Alcohol ◽  
Limit Of Detection ◽  
Good Resolution ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Gas Chromatographic Method ◽  
Ethyl Amine

Abstract Background A simple and sensitive gas chromatographic method was developed and validated for the simultaneous determination of methanol, ethanol, acetone, isopropyl alcohol, dichloromethane, N-hexane, ethyl acetate, tetrahydrofuran, and N,N-diisopropyl ethyl amine in Paclitaxel. A chromatographic separation was done on DB-624 column, 30 m length × 0.53 mm ID, and film thickness 3 μm, using a flame ionization detector (FID) with gradient column oven temperature program. The injection was carried out in split mode, with a split ratio of 5:1. A mixture of N-methyl-2-pyrrolidinone (contains 1% piperazine) and water in the ratio of 80:20 (v/v) was selected as a diluent to obtain good sensitivity along with the recovery. Results The developed gas chromatographic method offers symmetric peak shape, good resolution of more than 2.0 between the solvent peaks, and the relative standard deviation for replicate injections of all the solvents were found to be not more than 15.0% with reasonable retention time for all the solvents. The limit of detection for methanol, ethanol, acetone, isopropyl alcohol, dichloromethane, N-hexane, ethyl acetate, tetrahydrofuran, and N,N-diisopropyl ethyl amine was found to be 304.69 ppm, 497.98 ppm, 498.99 ppm, 504.49 ppm, 61.81 ppm, 30.07 ppm, 505 ppm, 73.05 ppm, and 2.09 ppm, respectively. Limit of quantitation of methanol, ethanol, acetone, isopropyl alcohol, dichloromethane, N-hexane, ethyl acetate, tetrahydrofuran, and N,N-diisopropyl ethyl amine was found to be 89.62 ppm, 146.47 ppm, 146.76 ppm, 148.38 ppm, 18.18 ppm, 8.84 ppm, 148.53 ppm, 21.49 ppm, and 0.62 ppm, respectively. Precision was found to be satisfactory. Linear in the range of LOQ to 150% level for all the solvents, and accuracy along with robustness, is performed, and acceptable results were obtained. Conclusion The proposed method was demonstrated to be simple, sensitive, specific, linear, precise, accurate, and robust, hence can be used to determine the residual organic solvents in Paclitaxel drug substance and drug product.

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