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lc and lc–ms/ms studies for the identification and characterization of degradation products of acebutolol

Journal of Pharmaceutical Analysis 2018年第6期8卷 357-365页

作者： Uday Rakibe Ravi Tiwari Anand Mahajan Vipul Rane Pravin Wakte Department of Chemical Technology Dr.Babasaheb Ambedkar Marathwada University Department of Pharmaceutical Sciences SVKM's NMIMS Department of Pharmaceutical Analysis Goa College of Pharmacy

The aim of the present investigation was to demonstrate an approach involving use of liquid chromatography(lc) and liquid chromatography-mass spectrometry(lc–ms) to separate, identify and characterize very small quantities of degradation products(DPs) of acebutolol without their isolation from the reaction mixtures. The drug was subjected to oxidative, hydrolytic, thermal and photolytic stress conditions as per International Conference on Harmonization(ICH) guideline Q1 A(R2). Among all the stress conditions the drug was found to be labile in hydrolytic(acidic & basic) and photolytic stress conditions, while it was stable in water-induced hydrolysis, oxidative and thermal stress conditions. A total of four degradation products were formed. A C18 column was employed for the separation of all the DPs on a gradient mode by using high-performance liquid chromatography(HPlc). All the DPs were characterized with the help of their fragmentation pattern and the masses obtained upon lc–ms/ms and msnanalysis. All the hitherto unknown degradation products were identified as 1-(2-(2-hydroxy-3-(isopropylamino)propoxy)-5-(amino)phenyl)ethanone(DP-I), N-(4-(2-hydroxy-3-(isopropylamino)propoxy)-3-acetylphenyl)acrylamide(DP-II), 1-(2-(2-hydroxy-3-(isopropylamino)propoxy)-5-(hydroxymethylamino)phenyl)ethanone(DP-III) and 1-(6-(2-hydroxy-3-(isopropylamino)propoxy)-2,3-dihydro-2-propylbenzo[d]oxazol-5-yl)ethanone(DP-IV). Finally the in-silico carcinogenicity and hepatotoxicity predictions of the drug and all the DPs were performed by using toxicity prediction softwares viz., TOPKAT, LAZAR and Discovery Studio ADMET. The results of in-silico toxicity studies revealed that acebutolol(0.967) and DP-I(0.986) were found to be carcinogenic, while acebutolol(0.490) and DP-IV(0.437) were found to be hepatotoxic.

关键词： Acebutolol Stress testing lc lc–ms/ms Degradation pathway In-silico toxicity

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Fast and sensitive lc–ms/ms method for the simultaneous determination of lisinopril and hydrochlorothiazide in human plasma

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Journal of Pharmaceutical Analysis 2017年第3期7卷 163-169页

作者： Jaivik V.Shah Priyanka A.Shah Priya V.Shah Mallika Sanyal Pranav S.Shrivastav Department of Chemistry School of Sciences Gujarat University Department of Pharmacy M.S.University Department of Chemistry St.Xavier's College

A sensitive and rapid liquid chromatography-tandem mass spectrometry(lc–ms/ms) method has been developed for the simultaneous determination of lisinopril(LIS) and hydrochlorothiazide(HCTZ) in human plasma using their labeled internal standards(ISs). Sample pre-treatment involved solid phase extraction on Waters Oasis HLB cartridges using 100 μL of plasma, followed by liquid chromatography on Hypersil Gold C_(18)(50 mm×3.0 mm, 5 μm) column. The analytes were eluted within 2.0 min using acetonitrile-5.0 m M ammonium formate, p H 4.5(85:15, v/v) as the mobile phase. The analytes and ISs were analyzed in the negative ionization mode and quantified using multiple reaction monitoring. The method showed excellent linearity over the concentration range of 0.50–250.0 ng/m L for both the analytes. The intra-batch and inter-batch precision(% CV) was ≤5.26% and their extraction recoveries were in the range of 96.6%–103.1%. Matrix effect evaluated in terms of IS-normalized matrix factors ranged from 0.97 to 1.03 for both the analytes. The validated method was successfully applied to determine the plasma concentration of the drugs using 10 mg lisinopril and 12.5 mg hydrochlorothiazide fixed dose formulation in 18 healthy Indian volunteers.

关键词： Lisinopril Hydrochlorothiazide lc–ms/ms Solid phase extraction Human plasma

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Validated lc–ms/ms method for determination of YH-8, a novel PKnB inhibitor, in rat plasma and its application to pharmacokinetic study

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Acta Pharmaceutica Sinica B 2015年第5期5卷 467-472页

作者： Qianqian Zhai Jing Pang Guoqing Li Congran Li Xinyi Yang Liyan Yu Yucheng Wang Jian Li Xuefu You Institute of Medicinal Biotechnology Chinese Academy of Medical Sciences and Peking Union Medical College Key Laboratory of Sustainable Development of Marine Fisheries Ministry of Agriculture Yellow Sea Fisheries Research Institute Chinese Academy of Fishery Sciences

(E)-Methyl-4-aryl-4-oxabut-2-enoate(YH-8) is a novel PKn B protein kinase inhibitor with good anti-tuberculosis activity. To evaluate its pharmacokinetics in rats, a sensitive and selective high performance liquid chromatography–tandem mass spectrometric(lc–ms/ms) method has been developed and validated for the quantification of YH-8 in rat plasma for the first time. Samples were pre-treated using a liquid–liquid extraction with ethyl acetate and the chromatographic separation was performed on a C18 column by gradient elution with methanol–water as the mobile phase. YH-8 was detected using a tandem mass spectrometer in positive selected reaction monitoring(SRM) mode. Method validation revealed good linearity over the range of1–500 ng/m L for YH-8 with a lower limit of quantification(LLOQ) of 1 ng/m L. Intra- and inter-day precision of YH-8 assay in rat plasma samples were 2.0%–6.8%, with accuracy of the method being 100.69%–106.18%.Stability test showed that when spiked into rat plasma, YH-8 was stable for 12 h at room temperature, for up to15 days at -70℃, and after three freeze-thaw cycles. Extracted samples were found to be stable over 12 h in an auto-sampler. The method was successfully applied to the pharmacokinetic study of YH-8 in rats after oral administration at 100 mg/kg and 200 mg/kg.

关键词： YH-8 lc–ms/ms Pharmacokinetics Rat plasma Method validation

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Highly sensitive lc–ms/ms method to estimate doxepin and its metabolite nordoxepin in human plasma for a bioequivalence study

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Journal of Pharmaceutical Analysis 2018年第6期8卷 378-385页

作者： Nirav P.Patel Mallika Sanyal Naveen Sharma Dinesh S.Patel Pranav S.Shrivastav Bhavin N.Patel Bio-Analytical Laboratory Cliantha Research India Ltd.BodakdevAhmedabad 380054GujaratIndia Kadi Sarva Viswavidyalaya Sector-15Ghandhinagar 382715GujaratIndia Department of Chemistry St.Xavier's CollegeNavrangpuraAhmedabad 380009GujaratIndia Department of Chemistry School of SciencesGujarat UniversityNavrangpuraAhmedabad 380009GujaratIndia

A selective, sensitive and rugged liquid chromatography–tandem mass spectrometry(lc–ms/ms) assay has been developed for the simultaneous determination of doxepin(Dox) and its pharmacologically active metabolite, nordoxepin(NDox) in human plasma. The analytes and their internal standards(IS)were extracted from 500 m L of human plasma by liquid-liquid extraction using methyl tert-butyl *** separation was achieved on Hypurity C8 column(100 mm ? 4.6 mm, 5 mm) using a mixture of acetonitrile-methanol(95:5, v/v) and 2.0 mM ammonium formate in 93:7(v/v) ratio. Detection was accomplished by tandem mass spectrometry in the positive ionization and multiple reaction monitoring acquisition mode. The protonated precursor to product ion transitions studied for Dox, NDox,and their corresponding ISs, propranolol and desipramine, were m/z 280.1-107.0, 266.0-107.0,260.1-116.1 and 267.1-72.1, respectively. A linear dynamic range of 15.0–3900 pg/mL for Dox and 5.00–1300 pg/mL for NDox was established with mean correlation coefficient(r2) of 0.9991 and 0.9993, respectively. The extraction recovery ranged from 86.6%–90.4% and 88.0%–99.1% for Dox and NDox, respectively. The intra-batch and inter-batch precision(% CV) across quality control levels was r 8.3% for both the analytes. Stability evaluated under different storage conditions showed no evidence of degradation and the % change in stability samples compared to nominal concentration ranged from 4.7% to12.3%. The method was successfully applied to a bioequivalence study of 6 mg doxepin hydrochloride orally disintegrating tablet in 41 healthy Indian subjects under fasting and fed conditions.

关键词： Doxepin Nordoxepin lc–ms/ms Liquid-liquid extraction Human plasma Bioequivalence study

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Application of an lc–ms/ms method for the analysis of amlodipine,valsartan and hydrochlorothiazide in polypill for a bioequivalence study

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Journal of Pharmaceutical Analysis 2017年第5期7卷 309-316页

作者： Jaivik V.Shah Jignesh M.Parekh Priyanka A.Shah Priya V.Shah Mallika Sanyal Pranav S.Shrivastav Department of Chemistry School of Sciences Gujarat University Department of Chemistry St.Xavier's College Department of Pharmacy M.S.University

A sensitive and selective method has been proposed for the simultaneous determination of amlodipine(AML),valsartan(VAL) and hydrochlorothiazide(HCTZ) in human plasma by liquid chromatography–tandem mass spectrometry(lc–ms/ms). The analytes and their deuterated analogs were quantitatively extracted from100 μL human plasma by solid phase extraction on Oasis HLB cartridges. The chromatographic separation of the analytes was achieved on a Chromolith RP18 e(100 mm × 4.6 mm) analytical column within 2.5 min. The resolution factor between AML and VAL, AML and HCTZ, and VAL and HCTZ was 2.9, 1.5 and 1.4, respectively,under isocratic conditions. The method was validated over a dynamic concentration range of 0.02–20.0 ng/m L for AML, 5.00–10,000 ng/m L for VAL and 0.20–200 ng/m L for HCTZ. Ion-suppression/enhancement effects were investigated by post-column infusion technique. The mean IS-normalized matrix factors for AML, VAL and HCTZ were 0.992, 0.994 and 0.998, respectively. The intra-batch and inter-batch precision(% CV) across quality control levels was ≤ 5.56% and the recovery was in the range of 93.4%–99.6% for all the analytes. The method was successfully applied to a bioequivalence study of 5 mg AML + 160 mg VAL + 12.5 mg HCTZ tablet formulation(test and reference) in 18 healthy Indian males under fasting. The mean log-transformed ratios of C max, AUC0–120 h and AUC0-inf and their 90% CIs were within 90.2%–102.1%. The assay reproducibility was demonstrated by reanalysis of 90 incurred samples.

关键词： Amlodipine Valsartan Hydrochlorothiazide lc–ms/ms Polypill Bioequivalence

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Comparison of ESI–and APCI–lc–ms/ms methods:A case study of levonorgestrel in human plasma

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Journal of Pharmaceutical Analysis 2016年第6期6卷 356-362页

作者： Rulin Wang Lin Zhang Zunjian Zhang Yuan Tian Key Laboratory of Drug Quality Control and Pharmacovigilance Ministry of EducationChina Pharmaceutical University State Key Laboratory of Natural Medicine China Pharmaceutical University

Electrospray ionization(ESI) and atmospheric pressure chemical ionization(APCI) techniques for liquid chromatography–tandem mass spectrometry(lc–ms/ms) determination of levonorgestrel were *** consideration of difference in ionization mechanism,the two ionization sources were compared in terms of lc conditions,ms parameters and performance of *** sensitivity for detection of levonorgestrel with ESI was 0.25 ng/m L which was lower than 1 ng/m L with *** effects were evaluated for levonorgestrel and canrenone(internal standard,IS) in human plasma,and the results showed that APCI source appeared to be slightly less liable to matrix effect than ESI *** an overall consideration,ESI was chosen as a better ionization technique for rapid and sensitive quantification of *** optimized lc–ESI–ms/ms method was validated for a linear range of 0.25–50 ng/m L with a correlation coefficient ≥*** intra-and inter-batch precision and accuracy were within 11.72% and 6.58%,*** application of this method was demonstrated by a bioequivalence study following a single oral administration of 1.5 mg levonorgestrel tablets in 21 Chinese healthy female volunteers.

关键词： Levonorgestrel lc–ms/ms Pharmacokinetics Electrospray ionization Atmospheric pressure chemical ionization

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A novel lc–ms/ms assay for methylprednisolone in human plasma and its pharmacokinetic application

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Asian Journal of Pharmaceutical Sciences 2016年第3期11卷 459-468页

作者： Sridhar Siddiraju Mercy Lazar Lal Prasanth Tadiboyina Sirisha Department of Pharmaceutical Chemistry Malla Reddy College of Pharmacy Osmania University Department of Pharmacy Shri Jagdishprasad Jhabarmal Tibrewala University Department of Pharmaceutical Chemistry JSS College of Pharmacy JSS University

Methylprednisolone is a synthetic glucocorticoid. In our report, the authors proposed a sensitive and selective liquid chromatography/tandem mass spectrometry(lc–ms/ms) assay for the determination of methylprednisolone applying budesonide as internal standard. Liquid–liquid extraction(LLE) having tert–butyl methyl ether(TBME) have been employed to extract methylprednisolone from the plasma samples. Immediately after reconstitution, the samples were chromatographed on a C18 column using an isocratic mobile phase composed of 10 m M ammonium formate buffer and acetonitrile(35:65, v/v). A flow rate of 1.00 ml/min was used to elute the analyte form the column. Analysis was carried out with an API–4000 lc–ms/ms instrument operated in multiple reaction-monitoring(MRM) mode. The linearity has been proven within the concentration range of 10.1–804 ng/ml in plasma samples. The precision(%CV) and accuracy results in five validation batches across five concentration levels were well within the acceptance limits. The drug was stable under different conditions. The particular assay has been proficiently put on pharmacokinetic study in healthy male subjects.

关键词： Methylprednisolone Human plasma Method validation lc–ms/ms Pharmacokinetics

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Determination of ifenprodil by lc–ms/ms and its application to a pharmacokinetic study in healthy Chinese volunteers

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Acta Pharmaceutica Sinica B 2013年第3期3卷 180-184页

作者： Jing Yang Chengtao Lu Wei Song Jiankang Li Yi Ding Yanrong Zhu Jinyi Cao Likun Ding Yanyan Jia Aidong Wen Department of Pharmacy Xijing HospitalFourth Military Medical UniversityShanxi 710032China

This paper reports the development and validation of an assay for ifenprodil based on liquid chromatography–tandem mass spectrometry(lc–ms/ms)and its application to a pharmacokinetic study involving single and multiple intravenous infusions to healthy Chinese *** sample preparation of plasma by liquid–liquid extraction with ethyl acetate,the analyte and internal standard,urapidil,were separated by reversed phase chromatography in a run time of 4 min and detected by positive ion electrospray ionization followed by multiple reaction monitoring of the precursor-to-product ion transitions at m/z 326.2-308.1 for ifenprodil and m/z 388.4-205.3 for *** assay was linear in the concentration range 0.2–50.0 ng/mL with recovery 476.4%.In the pharmacokinetic study of single intravenous infusions of 5,10 and 15 mg ifenprodil,peak plasma concentrations and areas under the plasma concentration–time curve were both linearly related to *** the pharmacokinetic study of multiple once daily intravenous infusions of 10 mg ifenprodil for 7 days,pharmacokinetic parameters were similar to those after the single dose showing that ifenprodil does not accumulate on repeated administration.

关键词： Ifenprodil Liquid/liquid extraction lc–ms/ms Pharmacokinetics Intravenous infusion Human Plasma

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Application of lc–ms/ms for quantitative analysis of glucocorticoids and stimulants in biological fuids

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Journal of Pharmaceutical Analysis 2013年第5期3卷 341-348页

作者： Jamshed Haneef Mohammad Shaharyar Asif Husain Mohd Rashid Ravinesh Mishra Shama Parveen Niyaz Ahmed Manoj Pal Deepak Kumar Department of Pharmaceutical Chemistry Faculty of Pharmacy Jamia Hamdard (Hamdard University) Department of Chemistry Indian Institute of Technology (IIT) Research Institute of Natural Sciences Department of Chemistry Changwon National University

Liquid chromatography tandem mass chromatography （lc-ms/ms） is an important hyphenated technique for quantitative analysis of drugs in biological fluids. Because of high sensitivity and selectivity, lc-ms/ms has been used for pharmacokinetic studies, metabolites identification in the plasma and urine. This manuscript gives comprehensive analytical review, focusing on chromatographic separation approaches （column packing materials, column length and mobile phase） as well as different acquisition modes （SIM, MRM） for quantitative analysis of glucocorticoids and stimulants. This review is not meant to be exhaustive but rather to provide a general overview for detection and confirmation of target drugs using lc-ms/ms and thus useful in the doping analysis, toxicological studies as well as in pharmaceutical analysis.

关键词： lc–ms/ms Ionization techniques Glucocorticoids Stimulants Hyphenated techniques Biological fuid

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Precolumn derivatization lc-ms/ms method for the determination and pharmacokinetic study of glucosamine in human plasma and urine

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Journal of Pharmaceutical Analysis 2012年第1期2卷 19-28页

作者： Min Songa, Tai-Jun Hanga, Cheng Wanga, Lin Yangb, Ai-Dong Wenb aDepartment of Pharmaceutical Analysis, China Pharmaceutical University, Nanjing 210009, China bDepartment of Pharmacy, Xijing Hospital, Xi’an 710032, China Department of Pharmaceutical Analysis China Pharmaceutical University Nanjing 210009 China. Department of Pharmacy Xijing Hospital Xi'an 710032 China.

A selective precolumn derivatization liquid chromatography–tandem mass spectrometric (lc–ms/ms) method for the determination of glucosamine in human plasma and urine has been developed and validated. Glucosamine was derivatized by o-phthalaldehyde/3-mercaptopropionic acid. Chromatographic separation was performed on a Phenomenex ODS column (150 mm 4.6 mm, 5 mm) using linear gradient elution by a mobile phase consisting of methanol (A), and an aqueous solution containing 0.2% ammonium acetate and 0.1% formic acid (B) at a flow rate of 1 mL/min. Tolterodine tartrate was used as the internal standard (IS). With protein precipitation by acetonitrile and then the simple one-step derivatization, a sensitive bio-assay was achieved with the lower limit of quantitation (LLOQ) as low as 12 ng/mL for plasma. The standard addition calibration curves suitable for clinical sample analysis showed good linearity over the range of 0.012–8.27 mg/mL in plasma and 1.80–84.1 mg/mL in urine. The fully validated method has been successfully applied to a pharmacokinetic study of compound glucosamine sulfate dispersible tablets in health Chinese volunteers receiving single oral doses at 500, 1000 and 1500 mg of glucosamine sulfate, as well as multiple oral doses of 500 mg t.i.d. for 7 consecutive days.

关键词： Glucosamine Pharmacokinetics Precolumn derivatization lc–ms/ms

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