Ultra-performance liquid chromatography/tandem mass spectrometry method for the determination of lercanidipine in human plasma

A simple, sensitive and rapid ultra-performance liquid chromatography/positive electrospray ionization tandem mass spectrometry (UPLC/ESI-MS/MS) method has been developed and validated for the determination of lercanidipine in human plasma. Lercanidipine and the internal standard, nicardipine, were extracted from plasma by liquid-liquid extraction using tert-butyl methyl ether as the extraction solvent. UPLC analysis was performed isocratically on an AcQuity UPLC BEH C18 analytical column (2.1 x 50.0 mm i.d., particle size 1.7 microm). The mobile phase consisted of 70% acetonitrile in water containing 0.2% v/v formic acid and pumped at a flow rate of 0.30 mL/min. ESI in positive ion mode, with multiple reaction monitoring (MRM), was chosen for the detection of the analytes. The assay was linear over a concentration range of 0.05-30 ng/mL for lercanidipine with a limit of quantitation of 0.05 ng/mL. Quality control samples (0.05, 0.15, 15 and 25 ng/mL) in five replicates from five of analytical runs demonstrated intra-assay precision (% CV < or =7.3%), inter-assay precision (% CV < or =6.1%) and an overall accuracy (% relative error) of less than 6.2%. A run time of less than 1.0 min for each sample made it possible to analyze a large number of human plasma samples per day. The method can be used to quantify lercanidipine in human plasma covering a variety of pharmacokinetic or bioequivalence studies.     

Ultra‐performance liquid chromatography‐tandem mass spectrometry method for the determination of febuxostat in dog plasma and its application to a pharmacokinetic study

A rapid, sensitive and selective ultra‐performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed and validated for the determination of febuxostat in dog plasma. Using paclitaxel as an internal standard (IS), a simple liquid–liquid extraction method with ethyl acetate was adopted for plasma sample pretreatment. Separation was carried out on an Acquity UPLC BEH C₁₈ column with a mobile phase consisting of acetonitrile and water (containing 0.2% formic acid). The assay was linear in the concentration ranged from 5 to 5000 ng/mL with a lower limit of quantification of 5 ng/mL for febuxostat. The single run analysis was as short as 2.0 min. Finally, the developed method was successfully applied to the pharmacokinetic study of febuxostat tablets following oral administration at a single dose of 40 mg in beagle dogs. Copyright © 2012 John Wiley & Sons, Ltd.     

An UPLC‐MS3 Method for Rapid Separation and Determination of Four Tobacco‐specific Nitrosamines in Mainstream Cigarette Smoke

An ultra‐high‐pressure liquid chromatography/MS³ (UPLC‐MS³) method has been developed and validated for the quantitative determination of four major TSNAs in mainstream cigarette smoke using MS³ scan mode on a hybrid triple quadrupole‐linear ion trap mass spectrometer. The new method combining the UPLC with MS³ scan mode offers decreased sample analysis time and good selectivity. After mainstream cigarette smoke was collected on a Cambridge filter pad, the particulate matter was extracted with ammonium acetate solution and analyzed by UPLC‐MS³ using isotopically labeled analogues as internal standards. Four TSNAs were completely separated on an Agilent XDB‐C₁₈ UPLC column using isocratic elution during a 6 min LC run time. Excellent linearity was obtained over the concentration range of 1.0‐150.0 ng/mL for all TSNAs with values for correlation coefficient (r) between 0.9985‐0.9994. Limits of detection (LOD) of each TSNA varied from 0.023 to 0.067 ng/mL, and lower limits of quantification (LLOQ) varied from 0.077 to 0.223 ng/mL, respctively. The recovery of each TSNA was from 89.2 to 106.8%. The method achieved excellent reproducibility with RSD 2.1‐6.8% for intra‐assay and 3.4‐9.1% for inter‐assay. This method can be used as an effective approach to significantly improve the detection capability for TSNAs in complex matrices.     

Detection of trace amounts of citrinin in dried orange peel by using an optimized extraction method coupled with ultra‐performance liquid chromatography–tandem mass spectrometry

A fast and sensitive method involving ultra‐performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) was introduced to detect citrinin in dried orange peel. A series of extraction, purification and chromatographic conditions was also systematically examined. With the proposed method, the obtained calibration graph was linear, with an R of 0.9996 within a concentration range of 0.5–10 ng/mL. The estimated limits of detection and quantification were 0.05 and 0.17 ng/mL, respectively. Under the selected conditions, the relative recoveries in different citrus products spiked with 1–10 ng/mL citrinin were 89.4–98.7% with RSDs of <2.5%. Compared with previously reported analytical methods, the newly developed UPLC–MS/MS method showed excellent sensitivity and good precision in detecting citrinin. The results indicated that it is a reliable and effective technique for the detection of trace citrinin in dried orange peel.     

Pharmacokinetic study of intraperitoneally administered troglitazone in mice using ultra-performance liquid chromatography/tandem mass spectrometry

A rapid and sensitive ultra-performance liquid chromatography/tandem mass spectrometry (UPLC/MS/MS) method was developed and validated for the determination of troglitazone in mouse plasma. Troglitazone and its internal standard (IS), rosiglitazone, were separated on an ACQUITY UPLC BEH C(18) column (1.7 microm particle size, 50 x 2.1 mm i.d.) by gradient elution with water and methanol at a flow rate of 0.5 mL/min. The cycle time of each analysis was 2.5 min. Rosiglitazone and troglitazone eluted at 1.13 and 1.57 min, respectively, and were chromatographically resolved from the ion suppression and enhancement zones due to the biological matrix effect. Quantitation of the analytes was performed in electrospray negative ionization mode (ESI -ve) using multiple reaction monitoring (MRM) experiments. The weighted (1/x) calibration curve was quadratic over the plasma concentration range 1-2500 ng/mL with a correlation coefficient (r(2)) of 0.9966. The limit of quantitation (LOQ) of troglitazone in mouse plasma was lower than 1 ng/mL. The inter- and intra-day variations of the assay were lower than 12.1%; the overall accuracy ranged from 86.4-110.2% and recovery from spiked plasma was more than 60%. The developed method was successfully applied to determine troglitazone in mouse plasma after intraperitoneal administration.     

Determination of quinapril and quinaprilat in human plasma by ultraperformance liquid chromatography–electrospray ionization mass spectrometry

A novel, specific and sensitive ultraperformance liquid chromatography tandem mass spectrometry (UPLC–MS/MS) method was developed for the simultaneous determination of quinapril and its active metabolite quinaprilat in human plasma. The method involves a simple, one‐step extraction procedure coupled with an Acquity UPLC? BEH C₁₈ column (100 × 2.1 mm, i.d., 1.7 µm) with isocratic elution at a flow‐rate of 0.2 mL/min and lisinopril as the internal standard. Detection was performed on a triple‐quadrupole tandem mass spectrometer in multiple reaction monitoring mode via electrospray ionization. Using 250 µL plasma, the methods were validated over the concentration range 5.010–500.374 ng/mL for quinapril and 10.012–1000 ng/mL for quinaprilat, with a lower limit of quantification of 5.010 ng/mL for quinapril and 10.012 ng/mL for quinaprilat. The intra‐ and inter‐day precision and accuracy were within 10.0%. The recovery was 85.8, 62.6 and 61.3% for quinapril, quinaprilat and lisinopril, respectively. Total run time was 3.0 min only. Copyright © 2008 John Wiley & Sons, Ltd.     

Simultaneous determination of udenafil and its active metabolite, DA-8164, in human plasma and urine using ultra-performance liquid chromatography-tandem mass spectrometry: application to a pharmacokinetic study

A rapid, sensitive, and simple ultra-performance liquid chromatography-tandem mass spectrometry (UPLC/MS/MS) method for the determination of udenafil and its active metabolite, DA-8164, in human plasma and urine using sildenafil as an internal standard (IS) was developed and validated. Udenafil, DA-8164 and IS from a 100 microL aliquot of biological samples were extracted by protein precipitation using acetonitrile. Chromatographic separation was carried on an Acquity UPLC BEH C(18) column (50 x 2.1 mm, i.d., 1.7 microm) with an isocratic mobile phase consisting of acetonitrile and containing 0.1% formic acid (75:25, v/v) at flow rate of 0.4 mL/min, and total run time was within 1 min. Detection and quantification was performed by the mass spectrometer using multiple reaction-monitoring mode at m/z 517 --> 283 for udenafil, m/z 406 --> 364 for DA-8164 and m/z 475 --> 100 for IS. The assay was linear over a concentration range of 1-600 ng/mL with a lower limit of quantification of 1 ng/mL in both human plasma and urine. The coefficient of variation of this assay precision was less than 13.7%, and the accuracy exceeded 92.0%. This method was successfully applied for pharmacokinetic study after oral administration of udenafil 100 mg to healthy Korean male volunteers.     

Determination of lovastatin in human plasma by ultra-performance liquid chromatography/electrospray ionization tandem mass spectrometry

A fast and sensitive ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of lovastatin in human plasma. With simvastatin as internal standard, sample pretreatment involved one-step extraction with n-hexane-methylene dichloride-isopropanol (20:10:1, v/v/v) of 0.5 mL plasma. Chromatographic separation was carried out on an Acquity UPLC BEH C(18) column with mobile phase consisting of acetonitrile-water (containing 5 mmol/L ammonium acetate; 85:15, v/v) at a flow-rate of 0.35 mL/min. The detection was performed on a triple-quadrupole tandem mass spectrometer by multiple reaction monitoring (MRM) via electrospray ionization source with positive mode. The analysis time was shorter than 1.7 min per sample. The standard curve was linear (r2>or=0.99) over the concentration range 0.025-50.0 ng/mL with a lower limit of quantification of 0.025 ng/mL. The intra- and inter-day precision values were below 11% and the accuracy (relative error) was within 6.0% at three quality control levels. This is the first method of MS with MRM coupled to UPLC for the determination of lovastatin, which showed great advantages of high sensitivity, selectivity and high sample throughput. It was fully validated and successfully applied to the pharmacokinetic study of lovastatin tablets in healthy Chinese male volunteers after oral administration.     

Development and validation of UPLC tandem mass spectrometry assay for separation of a phase II metabolite of ramipril using actual study samples and its application to a bioequivalence study

In this paper, we present a validated UPLC‐MS/MS assay for determination of ramipril and ramiprilat from human plasma samples. The assay is capable of isolating phase II metabolites (acylglucornides) of ramipril from in vivo study samples which is otherwise not possible using conventional HPLC conditions. Both analytes were extracted from human plasma using solid‐phase extraction technique. Chromatographic separation of analytes and their respective internal standards was carried out using an Acquity UPLC BEH C₁₈ (2.1 × 100 mm), 1.7 µm column followed by mass spectrometric detection using an Waters Quattro Premier XE. The method was validated over the range 0.35–70.0 ng/mL for ramipril and 1.0–40.0 ng/mL for ramiprilat. Copyright © 2010 John Wiley & Sons, Ltd.     

UPLC‐MS/MS determination of voriconazole in human plasma and its application to a pharmacokinetic study

A sensitive and rapid ultra performance liquid chromatography tandem mass spectrometry (UPLC‐MS/MS) method was developed to determine voriconazole in human plasma. Sample preparation was accomplished through a simple one‐step protein precipitation with methanol. Chromatographic separation was carried out on an Acquity UPLC BEH C₁₈ column using an isocratic mobile phase system composed of acetonitrile and water containing 1% formic acid (45:55, v/v) at a flow rate of 0.50 mL/min. Mass spectrometric analysis was performed using a QTrap5500 mass spectrometer coupled with an electrospray ionization source in the positive ion mode. The multiple reaction monitoring transitions of m/z 351.0 → 281.5 and m/z 237.1 → 194.2 were used to quantify voriconazole and carbamazepine (internal standard), respectively. The linearity of this method was found to be within the concentration range of 2.0–1000 ng/mL with a lower limit of quantification of 2.0 ng/mL. Only 1.0 min was needed for an analytical run. This fully validated method was successfully applied to the pharmacokinetic study after oral administration of 200 mg voriconazole to 20 Chinese healthy male volunteers. Copyright © 2014 John Wiley & Sons, Ltd.     

Simultaneous determination of thirteen main components and identification of eight major metabolites in Xuebijing Injection by UPLC/Q-TOF

An ultra performance liquid chromatographic method was used for the simultaneous identification and quantification of thirteen main components in Xuebijing Injection, including uridine, gallic acid, guanosine, danshensu, protocatechualdehyde, oxypaeoniflorin, hydroxysafflor yellow A, paeoniflorin, ferulic acid, safflor yellow A, senkyunolide I, senkyunolide H and salvianolic acid B. The chromatographic separation was performed on an Acquity UPLC BEH C₁₈ column (1.7-μm, 2.1 × 100 mm, i.d.) with a gradient elution of acetonitrile and 0.2% acetic acid at a flow rate of 0.4 mL/min. The method was validated for linearity (r ² > 0.9990), intra- and inter-day precision (RSD < 1.94%), accuracy (91.8–99.7%), recovery (96.8–103.8%), limits of detection (0.16–8.0 ng), and limits of quantification (0.54–26.8 ng). At least eight metabolites in prototype were found in rat plasma and urine after intravenous injection of 4 mL/kg doses of Xuebijing Injection. The proposed method could be utilized to qualify and control Xuebijing Injection to ensure its safety and efficacy in application.     

Pharmacokinetics and bioavailability of gelsenicine in mice by UPLC–MS/MS

Gelsenicine is an indole alkaloid isolated from Gelsemium elegans Benth. In recent years, the role of G. elegans Benth preparations in anti‐tumor, analgesic, dilatation and dermatological treatment has attracted attention, and it has been applied clinically, but it is easy to cause poisoning with its use. An UPLC–MS/MS method was established to determine the gelsenicine in mouse blood, and the pharmacokinetics of gelsenicine after intravenous (0.1 mg/kg) and intragastric (0.5 and 1 mg/kg) administration was studied. Deltalin was used as internal standard; a UPLC BEH C₁₈ column was used for chromatographic separation. The mobile phase consisted of acetonitrile and 10 mmol/L ammonium acetate (0.1% formic acid) with a gradient elution flow rate of 0.4 mL/min. Multiple reaction monitoring mode was used for quantitative analysis of gelsenicine in electrospray ionization positive interface. Proteins from mouse blood were removed by acetonitrile precipitation. A validation of this method was performed in accordance with the US Food and Drug Administration guidelines. In the concentration range of 0.05–100 ng/mL, the gelsenicine in the mouse blood was linear (r > 0.995), and the lower limit of quantification was 0.05 ng/mL. In the mouse blood, the intra‐day precision RSD was <12%, the inter‐day precision RSD was <15%, the accuracy ranged from 89.8 to 112.3%, the average recovery was >76.8%, and the matrix effect was between 103.7 and 108.4%, which meet the pharmacokinetic research requirements of gelsenicine. The UPLC–MS/MS method is sensitive, rapid and selective, and has been successfully applied to the pharmacokinetic study of gelsenicine in mice. The absolute bioavailability of gelsenicine is 1.13%.     

塑料玩具中酚类环境雌激素在模拟汗液和唾液中溶出行为研究

建立了快速溶剂萃取-超高效液相色谱法同时测定塑料玩具中5种环境雌激素(EES)的分析方法。将塑料玩具样品剪碎后,用二氯甲烷作溶剂经快速溶剂萃取、浓缩、过滤,用超高效液相色谱ACQUITY UPLC-BEHC18柱(50 mm×2.1 mm,1.7μm)分离,以乙腈-水为流动相,梯度洗脱,流速0.4 mL/min;检测波长200 nm,外标法定量。该方法回收率为93.7%～98.2%,测定结果的相对标准偏差为0.4%～2.1%(n=6),检出限为0.11～0.42ng/mL。此方法可作为测定塑料玩具中酚类环境雌激素的分析方法。     

UPLC‐MS/MS assay for the simultaneous quantification of carvedilol and its active metabolite 4′‐hydroxyphenyl carvedilol in human plasma to support a bioequivalence study in healthy volunteers

An ultra‐performance liquid chromatography–tandem mass spectrometry (UPLC‐MS/MS) method has been developed for the simultaneous determination of carvedilol and its pharmacologically active metabolite 4′‐hydroxyphenyl carvedilol in human plasma using their deuterated internal standards (IS). Samples were prepared by solid‐phase extraction using 100 μL human plasma. Chromatographic separation of analytes was achieved on UPLC C18 (50 × 2.1 mm, 1.7 µm) column using acetonitrile‐4.0 mm ammonium formate, pH 3.0 adjusted with 0.1% formic acid (78:22, v/v) as the mobile phase. The multiple reaction monitoring transitions for both the analytes and IS were monitored in the positive electrospray ionization mode. The method was validated over a concentration range of 0.05–50 ng/mL for carvedilol and 0.01‐10 ng/mL for 4′‐hydroxyphenyl carvedilol. Intra‐ and inter‐batch precision (% CV) and accuracy for the analytes varied from 0.74 to 3.88 and 96.4 to 103.3% respectively. Matrix effect was assessed by post‐column analyte infusion and by calculation of precision values (coefficient of variation) in the measurement of the slope of calibration curves from eight plasma batches. The assay recovery was within 94–99% for both the analytes and IS. The method was successfully applied to support a bioequivalence study of 12.5 mg carvedilol tablets in 34 healthy subjects. Copyright © 2013 John Wiley & Sons, Ltd.     

超高效液相色谱-质谱/质谱联用法测定人血浆中的辛伐他汀

建立了超高效液相色谱-质谱/质谱联用法(UPLC-MS/MS)测定人血浆中辛伐他汀的浓度。血浆样品经乙醚-正己烷-异丙醇(体积比为80∶20∶3)提取,以洛伐他汀为内标,采用ACQUITY UPLCTM BEH C18柱(50 mm×2.1 mm,1.7 μm)分离,以乙腈-10 mmol/L乙酸铵水溶液(体积比为85∶15)为流动相,流速为0.25 mL/min,通过电喷雾离子化,采用多反应监测(MRM)方式进行正离子检测。线性范围为0.051～20.4 ng/mL,日内及日间测定的相对标准偏差不高于10%,平均回收率为91.6%。方法灵敏度高,分析速度快,操作简便,适用于辛伐他汀药物动力学和生物等效性研究。     

A novel,rapid and sensitive UPLC–MS/MS method for the determination of macitentan in patients with pulmonary arterial hypertension

Macitentan is an endothelin receptor antagonist commonly used in the treatment of pulmonary arterial hypertension (PAH). A novel, rapid, simple and sensitive UPLC–MS/MS method was developed and validated for pharmacokinetic study and the determination of macitentan in PAH patients. Macitentan and bosentan, which are used as internal standards, were detected using atmospheric pressure chemical ionization in positive ion and multiple reaction monitoring mode by monitoring the mass transitions m/z 589.1 → 203.3 and 552.6 → 311.5, respectively. Chromatographic separation was performed on a reverse‐phase C18 column (5 μm, 4.6 × 150 mm) with an isocratic mobile phase, which consisted of water containing 0.2% acetic acid–acetonitrile (90:10, v/v) at a flow rate of 1 mL/min. Retention times were 1.97 and 1.72 min for macitentan and IS, respectively. The calibration curve with high correlation coefficient (0.9996) was linear in the range 1–500 ng/mL. The lower limit of quantitation and average recovery values were determined as 1 ng/mL and 89.8%, respectively. This method is the first UPLC–MS/MS method developed and validated for the determination of macitentan from human plasma. The developed analytical method was fully validated for linearity, selectivity, specificity, accuracy, precision, sensitivity, stability, matrix effect and recovery according to US Food and Drug Administration guidelines. The developed method was applied successfully for pharmacokinetic study and the determination of macitentan in PAH patients.     

Simultaneous determination of the bioactive components in rat plasma by UPLC‐MS/MS and application in pharmacokinetic studies after oral administration of radix Scutellariae extract

A highly sensitive and rapid ultraperformance liquid chromatography–tandem mass spectrometry (UPLC‐MS/MS) method has been developed and validated for simultaneous quantification of the four main bioactive compounds, i.e. baicalin, baicalein, wogonoside and wogonin, in rat plasma after oral administration of Radix Scutellariae extract. Clarithromycin was used as an internal standard (IS). Plasma samples were processed by protein precipitation with methanol. The separation was performed on an Acquity BEH C₁₈ column (100 × 2.1 mm, 1.7 μm) at a flow rate of 0.4 mL/min, using 0.1% formic acid–acetonitrile as mobile phase. The MS/MS ion transit ions monitored were 447.5 → 270.1 for baicalin, 270.1 → 168.1 for baicalein, 461.2 → 284.0 for wogonoside, 284.2 → 168.1 for wogonin and 748.5 → 158.1 for IS. Method validation was performed according to US Food and Drug Administration guidelines and the results met the acceptance criteria. The lower limit of quantification (LLOQ) achieved was 1.13 ng/mL for baicalin, 1.23 ng/mL for baicalein, 0.82 ng/mL for wogonoside and 0.36 ng/mL for wogonin. The calibration curves obtained were linear (r > 0.99) over the concentration range ~ 1–1000 ng/mL. The intra‐ and inter‐day precision was <15% and the accuracy was within ±14.7%. After validation, this method was successfully applied to a pharmacokinetic study of Radix Scutellariae extract.     

Validation of an ultra‐performance liquid chromatography–tandem mass spectrometry method for the determination of flecainide in human plasma and its clinical application

A simple and reproducible bioanalytical method for the determination of flecainide in human plasma was developed and validated using an ultra‐performance liquid chromatography with tandem mass spectrometry (UPLC‐MS/MS) to obtain higher sensitivity than the current available methods. After simple protein precipitation, flecainide and a stable isotope‐labeled internal standard (IS) were chromatographed on an Acquity UPLC BEH C₁₈ column (2.1 × 100 mm, 1.7 µm) with isocratic elution of mobile phase consisting of 45% methanol containing 0.1% formic acid at a flow rate 0.25 mL/min. Detection was performed in positive electrospray ionization by monitoring the selected ion transitions at m/z 415.4/301.1 for flecainide and m/z 419.4/305.1 for the IS. The method was validated according to current bioanalytical method validation guidelines. The calibration standard curve was linear from 2.5 to 1000 ng/mL using 0.1 mL of plasma. No significant interferences were detected in blank human plasma. Accuracy and precision in the intra‐ and inter‐batch reproducibility study were within acceptance criteria. Neither hemolysis effects nor matrix effects were observed. The UPLC‐MS/MS method developed was successfully applied to determine plasma flecainide concentrations to support clinical studies and incurred sample reanalysis also ensured the reproducibility of the method. Copyright © 2015 John Wiley & Sons, Ltd.     

Use of 18O3-clodronate as an internal standard for the quantitative analysis of clodronate in human plasma by gas chromatography/electron ionisation mass spectrometry

A sensitive and specific method for the quantitative determination of clodronate in human plasma is presented. The drug was extracted from plasma by anion-exchange chromatography and derivatised to the tetra-tert-butyldimethylsilyl derivative. 18O3-Clodronate was prepared from unlabeled clodronate and used as an internal standard. Gas chromatography/mass spectrometry (GC/MS) under electron ionisation conditions was used for quantitative measurement of the drug, using m/z 643.16 and 651.17 for target and internal standard, respectively. Calibration graphs were linear within the range of 10-1280 ng/mL plasma. Intra-day precision was 1.8% (10 ng/mL), 0.5% (40 ng/mL), 1.0% (120 ng/mL), 0.5% (200 ng/mL), 0.5% (400 ng/mL) and 2.7% (800 ng/mL) and inter-day variability was found to be 0.7% (10 ng/mL), 1.6% (40 ng/mL), 1.3% (120 ng/mL), 2.3% (200 ng/mL), 2.5% (400 ng/mL) and 1.2% (800 ng/mL). Intra-day accuracy showed deviations of 0.8% (10 ng/mL), 0.8% (40 ng/mL), 0.9% (120 ng/mL), 0.9% (200 ng/mL), 1.9% (400 ng/mL) and 0.3% (800 ng/mL) and intra-day accuracy was of -1.4% (10 ng/mL), 0.0% (40 ng/mL), -0.7% (120 ng/mL), -0.4% (200 ng/mL), -1.2% (400 ng/mL) and -3.3% (800 ng/mL). The stable isotope labeled standard was found to be stable under analysis conditions.     

超高效液相色谱-三重四极杆质谱联用方法测定血浆和尿液中的α-龙葵碱、α-卡茄碱和茄啶

建立了超高效液相色谱-三重四极杆质谱联用方法,检测血浆和尿液中的α-龙葵碱、α-卡茄碱和茄啶。样品经2%(v/v,下同)甲酸水溶液等量稀释,再经混合型阳离子交换固相萃取柱(MCX SPE)净化,以0.1%甲酸乙腈溶液和含0.05%甲酸的5 mmol/L乙酸铵水溶液作为流动相进行梯度洗脱,在UPLC BEH C18色谱柱上实现分离,正离子电喷雾串联质谱多反应监测(ESI-MS/MS MRM)方式检测,基质匹配外标法定量。一次进样分析时间为5.5min。血浆和尿液中3种待测物的线性范围均为0.3~100 ng/mL,相关系数为0.997~0.999;样品的检出限为0.1 ng/mL,定量限为0.3 ng/mL;血浆和尿液中的平均加标回收率分别为82%~112%和96%~114%,相对标准偏差为4.0%~16%和2.7%~17%(n=6)。方法简单、准确、灵敏,适用于马铃薯中毒检测。