scholarly journals Simultaneous determination of seven glucocorticoids in cosmetics by liquid chromatography tandem mass spectrometry

Author(s):  
Dong Bui Quang ◽  
Phuong Vu Thi ◽  
Van Anh Tran Thi ◽  
Son Tran Cao ◽  
◽  
...  

A rapid high-performance liquid chromatography method with electrospray ionization and tandem mass spectrometry detection (LC-ESI-MS/MS) was developed and validated for the simultaneous determination of 7 glucocorticoids (GC) including hydrocortisone acetate (HCA), cortisone acetate (COA), prednisone (PDS), prednisolone (PDL), methyl prednisolone (MPL), dexamethasone (DEX) and fluocinolone acetonide (FLA), which may be illegally blended in transdermal cosmetics. Sample preparation step consists of the extraction with ethyl acetate followed by centrifugation and filtration. The extract was dried, diluted and cleaned using C18 SPE column. The compounds were separated by reversed-phase chromatography with mobile phase containing 0.1% formic acid in water and acetonitrile in gradient condition. The method was validated at the validation level from 0.12 to 6.0 µg/g. The LODs for PDS, PDL and FLA were 0.3 µg/g and for the others were 0.03 µg/g, and LOQs were 0.6 and 0.12 µg/g, respectively. The reproducibility was satisfied with the relative standard deviation below 23% and the recoveries were in the range of 74.3-106.7% meeting AOAC requirements. The studied glucocorticoids were detected in about 20% of tested samples collected in Hanoi with the level contents in the range from 0.18 to 16.2 µg/g.

2007 ◽  
Vol 90 (1) ◽  
pp. 343-348 ◽  
Author(s):  
Ross A Potter ◽  
B Garth Burns ◽  
Jeffrey M van de Riet ◽  
David H North ◽  
Rozina Darvesh

Abstract A simple, robust method using liquid chromatography/tandem mass spectrometry (LC/MS/MS) for the simultaneous determination of 17 sulfonamides sulfanilamide (SNL), sulfacetamide (SAA), sulfaguanidine (SGD), sulfapyridine (SPY), sulfadiazine (SDZ), sulfathiazole (STZ), sulfamerazine (SMR), sulfamethoxazole (SOZ), sulfamoxole (SXL), sulfisoxazole (SXZ), sulfamethizole (SML), sulfamethazine (SMZ), sulfamethoxypyridazine (SMP), sulfamonomethoxine (SMM), sulfachloropyridazine (SCP), sulfaquinoxaline (SQX), and sulfadimethoxine (SDM) and 2 potentiators ormetoprim (OMP) and trimethoprim (TMP) in fish tissue has been developed. The analytes were extracted from homogenized fish tissue with wateracetonitrile (50 + 50). The extract was clarified by centrifugation and a portion defatted with hexane. The analytes were partitioned into chloroform and evaporated to dryness. The redissolved residue was applied to a C18 reversed-phase column with a wateracetonitrile (0.1% acetic acid) gradient. All of the compounds were completely separated and detected in <10 min at 30°C using LC/MS/MS. Standard curves were linear over the range of 0.02 to 5 ng injected. The limit of detection varied from 0.1 ng/g for SMZ and OMP to 0.9 ng/g for SXL and SOZ. Recoveries varied from 100% for SDM, SOZ, and SQX and 85% for SMR, OMP, and TMP to approximately 30% for SAA. Relative standard deviations for repeat analysis varied from 4% for SMZ and SCP to 23% for SAA.


Molecules ◽  
2020 ◽  
Vol 25 (5) ◽  
pp. 1254 ◽  
Author(s):  
Won-Gu Choi ◽  
Dong Kyun Kim ◽  
Yongho Shin ◽  
Ria Park ◽  
Yong-Yeon Cho ◽  
...  

Doxorubicin, an anthracycline antitumor antibiotic, acts as a cancer treatment by interfering with the function of DNA. Herein, liquid chromatography-tandem mass spectrometry was for the first time developed and validated for the simultaneous determination of doxorubicin and its major metabolites doxorubicinol, doxorubicinone, doxorubicinolone, and 7-deoxydoxorubicinone in mouse plasma. The liquid–liquid extraction of a 10 μL mouse plasma sample with chloroform:methanol (4:1, v/v) and use of the selected reaction monitoring mode led to less matrix effect and better sensitivity. The lower limits of quantification levels were 0.5 ng/mL for doxorubicin, 0.1 ng/mL for doxorubicinol, and 0.01 ng/mL for doxorubicinone, doxorubicinolone, and 7-deoxydoxorubicinone. The standard curves were linear over the range of 0.5–200 ng/mL for doxorubicin; 0.1–200 ng/mL for doxorubicinol; and 0.01–50 ng/mL for doxorubicinone, doxorubicinolone, and 7-deoxydoxorubicinone in mouse plasma. The intra and inter-day relative standard deviation and relative errors for doxorubicin and its four metabolites at four quality control concentrations were 0.9–13.6% and –13.0% to 14.9%, respectively. This method was successfully applied to the pharmacokinetic study of doxorubicin and its metabolites after intravenous administration of doxorubicin at a dose of 1.3 mg/kg to female BALB/c nude mice.


2020 ◽  
Vol 2020 ◽  
pp. 1-7
Author(s):  
Dinh-Vu Le ◽  
Trong-Tuan Nguyen ◽  
Van-Trong Nguyen

A liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method has been validated for the simultaneous determination of methamphetamine (MA) and 3,4-methylenedioxy-N-methamphetamine (MDMA) in the blood sample. Under the optimal experimental conditions, the concentration of MA can be determined in the range from 1 µg/L to 5000 µg/L with the method detection limit (MDL) of 0.31 µg/L. The range from 0.5 to 500 µg/L is observed for the determination of MDMA with the MDL down to 0.25 µg/L. The practical applicability of the method is performed with the recovery ranging from 85.3% to 94% for MA and from 86.9% to 95.5% for MDMA. At the different concentrations of drugs, the relative standard deviations (RSD) for both MA and MDMA are lower than 5.7%. The method was applied to analyse 1995 blood samples that had been collected from the Forensic Medicine Centre of Ho Chi Minh City. The results showed 1.75% positive with MA and 0.25% positive with MDMA. These two drugs take 10% of the total drugs positive samples. By using deuterium-labelled methamphetamine-d5 and 3,4-methylenedioxy-N-methamphetamine-d5 as the internal standards in the determination and the use of MS/MS in multiple reaction monitoring mode signal readout, the method exhibits robustness specificity and can be applied in simultaneous determination of MA and MDMA in blood with high selectivity and sensitivity.


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