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@#A quantitative analysis method based on solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS) for simultaneous determination of illicit drugs and their metabolites in wastewater was established. Samples filtered at pH of 2 and spiked with internal standard were loaded to Oasis Prime MCX cartridges for solid-phase extraction. The samples were washed with 4 mL of methanol and eluted with 4 mL of 5% ammonia in acetonitrile before reconstituting with 0.1% formic acid/water solution. ZORBAX Eclipse Plus C18 column was used for chromatography, and gradient elution was performed with 0.1% formic acid/water solution and acetonitrile as mobile phase. The samples were then detected by electrospray ionization (ESI) in positive ion mode, and multiple reaction monitoring mode (MRM) was adopted for quantitative analysis. All analytes had a good linear relationship (r ≥ 0.993 2) within the range of their respective standard curve; the limit of quantification was 1 ng/L (except amphetamine at 2.5 ng/L); the extraction recovery ranged from 82.13% to 99.96%; and the intra- and inter-day precisions were less than 9.43%. The method is accurate, reliable and reproducible, and is suitable for the quantitative determination of illicit drugs and their metabolites in wastewater and can provide an analytical method for real-time monitoring of drug abuse.
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Abstract@#Polycyclic aromatic hydrocarbons (PAHs) are ubiquitous pollutants with toxic effects and adverse health impacts on general population. Several methods of extraction had been applied to extract PAHs from human blood samples such as solid phase extraction (SPE). The SPE represents one of the most common techniques for extraction and clean-up procedures as it needs low quantity of solvents with less manual efforts. Similarly, various analytical instruments like gas chromatography coupled to mass spectrometry (GC-MS) was used to measure the PAHs levels. Gas chromatography is a simple, fast, and very efficient method for solvents and small organic molecules. This review provides an overview of the measured concentrations of PAHs in human blood samples through the application of SPE and GCMS during the last ten years. While these studies used various solvents, their application of SPE method and GC-MS revealed rewarding results about the determination of PAHs levels in the human samples.
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@#Introduction: Bisphenol A (BPA) is a controversial plastics ingredient used mainly in the production of polycarbonate plastics (PC) and epoxy resins that widely used nowadays in food and drink packaging. Even though BPA is not involved in polyethylene terephthalate (PET) manufacturing, recent study had reported the present of BPA in PET water bottle. This study was conducted to investigate effects storage conditions on release of BPA from PC and PET bottled water as well as to assess health risks associated with consumption. Methods: Solid phase extraction (SPE) was used to extract the samples, followed by analysis using ultra high performance liquid chromatography with fluorescence detector (UHPLC-FLD). The possibility of developing chronic non-carcinogenic health risk among consumers of bottled water was evaluated using hazard quotient (HQ). Results: Results showed that BPA migrated from PC and PET water bottles at concentrations ranging from 9.13 to 257.67 ng/L and 11.53 ng/L to 269.87 ng/L respectively. Concentrations of BPA were higher in PET bottled water compared to PC bottled water across all storage conditions. Higher storage temperature and longer storage duration increased BPA concentrations in PC and PET bottled water. Concentrations of BPA in bottled water which were kept in a car and were exposed to sunlight were higher than control samples which were stored indoor at room temperature. Conclusion: No significant chronic non-carcinogenic health risks were calculated for daily ingestion of BPA-contaminated bottled water; calculated HQ was less than one.
Subject(s)
Risk AssessmentABSTRACT
An analytical method based on ultra-performance liquid chromatography with positive ion electrospray ionization (ESI) coupled with tandem mass spectrometry (UPLC–MS/MS) was developed and validated for the determination of therapeutic peptide desmopressin in human plasma. A desmopressin stable labeled isotope (desmopressin d8) was used as an internal standard. Analyte and the internal standard were extracted from 200 μL of human plasma via solid-phase extraction technique using Oasis WCX cartridges. The chromatographic separation was achieved on an Aquity UPLC HSS T3 column by using a gradient mixture of methanol and 1 mM ammonium formate buffer as the mobile phase. The calibration curve obtained was linear (r2≥0.99) over the concentration range of 1.01–200 pg/mL. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. The results of the intra- and inter-day precision and accuracy studies were well within the acceptable limits. The proposed method was successfully applied to pharmacokinetic studies in humans.
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El consumo de drogas de síntesis ha ido en aumento. Estos nuevos derivados sintéticos son análogos estructurales de la feniletilamina N-sustituida. Este grupo ha provocado severos casos de intoxicación e incluso probablemente la muerte de varios consumidores. El principal derivado es conocido como 25C-NBOMe y se consume en estampillas idénticas al LSD. En este trabajo se desarrolla una metodología analítica para la determinación de 25C-NBOMe mediante cromatografía planar instrumental (cromatografía en capa delgada de alta resolución) y cromatografía de gases con detector de masas (CG/EM) como técnicas alternativas de fácil manejo y costo. Estas metodologías demostraron ser robustas y confiables para el propósito previsto.
Consumption of synthetic drugs has increased. These new synthetic derivatives are structural analogs of N-substituted phenylethylamine, and this group has caused severe cases of poisoning and even probably the death of several users. The main derivative is known as 25C-NBOMe and it is consumed in blotters in the same manner as LSD. In this work, an analytical methodology for 25C-NBOMe determination by instrumental planar chromatography high-performance thin-layer chromatography (HPTLC) and gas chromatography with mass detector (GC/MS) were developed as alternative techniques; they are easy to use and low cost. These methods proved to be robust and reliable for the intended purpose.
O consumo de drogas sintéticas vem aumentando. Esses novos derivados sintéticos são análogos estruturais de feniletilamina N-substituída, este grupo tem causado casos graves de intoxicação e, até mesmo, provavelmente, a morte de vários consumidores. O principal derivado é conhecido como 25C-NBOMe e consumido em selos idênticos ao LSD. Neste trabalho é desenvolvida uma metodologia analítica para a determinação de 25C-NBOMe através de cromatografia planar instrumental (cromatografia em camada delgada de alta resolução) e cromatografia gasosa com detector de massas (CG/EM) como técnicas alternativas de fácil utilização e custo. Estas metodologias demonstraram serem robustas e fiáveis para a finalidade a que se destinam.
Subject(s)
Humans , Urine , Chromatography , Hallucinogens , Chromatography, Gas , Solid Phase ExtractionABSTRACT
OBJECTIVE: To establish a Carb/NH2-SPE-GC-MS method for rapid monitoring of 40 kinds of pesticides of four categories in Toddaliae asiaticae (L.) Lam. METHODS: The samples were pretreated with Carb/NH2 solid phase extraction (SPE) subpost, and a GC-MS method was used for the determination of the trace pesticide residues. RESULTS: In comparison with the pesticide residue pretreatment methods included in the Chinese Pharmacopoeia, the Carb/NH2-SPE-GC-MS method showed no significant differences (P>0.05) and was simpler and more feasible in handling a variety of pesticide residues in Toddaliae asiaticae (L.) Lam. Good linearity was obtained for the calibration curves for the 40 kinds of pesticides in the concentration range of 10 to 200 ng·mL-1 (r>0.998 2), the limits of detections (LODs) were around 2.5 ng·mL-1, and the precisions, stabilities and recoveries basically met the methodological requirements. CONCLUSION: Carb/NH2-SPE-GC-MS method established in this paper is simple, rapid, highly sensitive, and accurate for the qualitative and quantitative analysis of multi-component pesticide residues in Toddaliae asiaticae (L.) Lam.
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OBJECTIVE: To establish a novel and efficient method for enriching low content active components from traditional Chinese herbs. METHODS: The enrichment of atractylenolide III was taken as an example. First, molecular imprinting polymers (MIPs) of atractylenolide III were prepared by precipitation polymerization using 1-Vinylimidazole as functional monomer. Second, the atractylenolide III MIPs were packed into solid-phase column to separate atractylenolide III and its analogues from the exracts of Herba Atractylodes Macrocephaia and Codonopsis pilosula. Moreover, the adsorption performance of MIPs for the target components was also investigated. RESULTS: Enrichment factor (EF) of MIP-SPE and C18-SPE column were 78.90 and 51.56 μg · g-1 respectively, suggesting that MIPs had better adsorption property than C18; the precision and accuracy of the developed method were satisfactory with recoveries of 102.2% and LOD of 0.36 μg · mL-1. CONCLUSION These results demonstrate the feasibility of molecularly imprinted solid phase extraction for enriching low content active components in traditional Chinese herbs.
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Objective: A novel method for the analysis of alkaloids in Nelumbo nucifera leaves was established by SPE-RRLC-Q-TOF mass spectrometry. Methods: The crude sample was extracted by 1% HCl with ultrasound-assisted extraction, then purified by SPE column, and eluted with ammonia-methanol (5:95). After concentration, the residue was dissolved by methanol solution. The real sample was analyzed by RRLC-Q-TOF. A Welch Materials C18 column was applied in the RRLC separation using acetonitrile and water as mobile phase. The elutes were detected by Q-TOF to obtain the MS spectra with extract molecular weights under positive ion mode. Results: Nine alkaloids were identified. Conclusion: This method can be used to rapidly determine the alkaloids of N. nucifera leaves.
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Objective:To establish a method for madecassoside determination by solid-phase extraction RP-HPLC in SD rats plasma. Methods:The sample was cleaned with an Strata-X solid-phase extraction . HPLC conditions were as follows:Welchrom-C18 column (250 mm?4.6 mm,5 ?m),water-acetonitrile(24∶76)as mobile phase(flowrate:1.0 ml/min),cucurbitacin B as internal standard, detection wavelength of 225 nm,and column temperature of 30℃. Results:In this situation,the remaining times of the madecassoside and cucurbitacin B were 5.11 min and 8.14 min,respectively. The linear range of the method was 5 ?g/ml～1.5 mg/ml (r=0.999 8).The low limit of detection was 1 ?g/ml. The method recoveries and the extraction recoveries were 90.21%～95.65% and 80.65%～87.04%,respectively. The within-day RSD and between-day RSD were between 1.31%～3.07%(n=5). Conclusion:Themethod is simple,convenient,accurate, reproducible,and suitable for studying the pharmacokinetics of madecassoside in SD rats .
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OBJECTIVE:To estabilish a HPLC-MS method for determining enalapril in human plasma METHODS:Alprozalam was added into plasma sample as an internal standard,then supernate of the sample was extracted through solid-phase extration column,washed with methanol and detected by HPLC-MS method:column,ODS C18;mobile phase,methanol-0 01% formic acid(45∶55);flow rate,0 8ml/min;capillary voltage,3 81kV;cone voltage,39 0V The selected ion was determined by EST RESULTS:The calibration curve was linear within the range of 2 5～400ng/ml r=0 9 996,the recovery was 102 2%,RSDs of intra -day and inter-day were 4 0% and 5 4%,respectively CONCLUSION:The method is accurate and sensitive with no endogenous interference It can be applied to studying the pharmacokinetics and bioavailability of enalapril tablets in humans
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Objective: To establish the method for determination of taurocholic acid in the Traditional Chinese Medicine Shedanchuanbei Oral Liquid and snake bile. Methods: The sample was prepared as mixed solution containing methanol and KH 2PO 4. The mixed solution was injected into Sep Pak C 18 cartridge for the purpose of sample purity. In this processing, the substances which having strong retain action and could harm analytic column were hold in the Sep Pak C 18 cartridge. The eluting solution that the Sep Pak C 18 cartridge had be over loading for taurocholic acid was used as the test solution. The test solution was measured by RP HPLC. The chromatographic conditions were as followed: Supelcosil LC 8 column(150mm?4.6nm,5?m) as analytic column, detect wavelength at 203nm, and MeOH 0.4%KH 2PO 4 mixed solution(56∶44, V/V ) as mobile phase. The inject volume was 50?L. Results: The linear response range of sodium taurocholate was from 0.0253mg?mL -1 to 0.253mg?mL -1 , and the correlation coefficient was 0.9999. The average recovery rate was 101.3%, RSD was 0.40%( n =6). Conclusion: This method was simple, efficient and suitable to the quality control for Shedanchuanbei Oral Liquid and snake bile.
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AIM: To determine the low content of Ophiopogon japonicus saponin metabolite in vivo. METHODS: HPLC-MS method of determining rat's metabolite diosgenin in vivo was established after single-dose oral Ophiopogon japonicus saponin enteric microsphere. RESULTS: The detection limit was about 50 ng/mL,Linearity,precision of intra and inter-day and reproducibility of the method were good. CONCLUSION: This method accords with the analysis requirement.It can give an effective measure and foundation for studying TCM saponin bioavailability.
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Objective: To determine tetrahydropalmatine in Juyanbaokang Granules (Rhizoma Corydalis, Radix Aconcti Lateralis Preparata, Radix Rauwolfiae, etc.) by SPE-HPLC. Methods : Samples were purified by C 18 SPE column. HPLC column was Dikma Diamonsil C 18 (250mm?4.6mm,5?m), mobile phase was 0.05M potassium dihydrogen phosphate-0.005M sodium heptanesulfonate-acetonitrile (1.2∶1.2∶1), flow rate was 1.2 mL?min -1 and detection wavelength was 230nm. Results : The calibration curve was linear in the range of 0.067 ～0.402?g for tetrahydropalmatine ( r =0.9997). The average recovery was 98.66%. Conclusion : The method with good separation is convenient, rapid, accurate and reliable.