在线样品前处理大体积进样离子色谱法直接测定海水中亚硝酸盐、硝酸盐和磷酸盐

采用戴安公司谱睿(Pre)在线样品除氯技术,结合OnGuard Ba柱去除硫酸盐,建立了离子色谱直接测定海水中亚硝酸盐、硝酸盐和磷酸盐的方法。该方法以IonPac AG23为富集柱,高容量IonPac AS23为分离柱,淋洗液自动发生装置在线产生KOH溶液进行梯度淋洗,抑制电导检测。实验结果表明: 样品稀释5～10倍时,直接进样不会干扰目标物测定。当流速为1 mL/min、进样量为500 μL时,海水中NO~2-N、NO~3-N、PO3~4-P的方法检出限分别为0.3、0.4、0.2 μg/L,线性范围分别为10～500 μg/L、14～680 μg/L、3.4～170 μg/L,线性相关系数r均大于0.9990。测得人工海水样品中目标物的加标回收率为92%～106%,相对标准偏差(RSD, n=6)为1.2%～7.7%。该方法一次进样可在13 min内完成分析,具有操作简单快捷、无污染等优点,能满足近海海水中NO~2、NO~3、PO3~4的定量分析要求。     

Determination of fluvoxamine in rat plasma by HPLC with pre-column derivatization and fluorescence detection using 4-fluoro-7-nitro-2,1,3-benzoxadiazole

A sensitive, simple and reliable method using high-performance liquid chromatographic (HPLC) assay of fluvoxamine (FLU), a selective serotonin reuptake inhibitor (SSRI), in rat plasma after pre-column derivatization with 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) was developed in this study. Extracted plasma samples were mixed with NBD-F at 60 degrees C for 5 min and injected into HPLC. Retention times of FLU and an internal standard (propafenone) derivative were 15.5 and 13.5 min, respectively. The calibration curve was linear over the range 0.015-1.5 microg/mL (r2 = 0.9985) and the lower limits of detection and quantification of FLU were 0.008 and 0.015 microg/mL, respectively, in 100 microL of plasma. The derivative sample was stable at 4 degrees C for 1 day. The coefficients of variation for intra-day and inter-day assay of FLU were less than 8.3 and 9.6%, respectively. Other SSRIs and centrally acting drugs did not interfere with the peak of the FLU derivative. The method was applied for analysis of the plasma samples from rats treated with FLU. These results indicate that the method presented is useful to determine the FLU levels in rat plasma of volumes as small as 100 microL and can be applied to pharmacokinetic studies.     

Simultaneous quantification of polar and non-polar volatile organic compounds in water samples by direct aqueous injection-gas chromatography/mass spectrometry

A direct aqueous injection-gas chromatography/mass spectrometry (DAI-GC/MS) method for trace analysis of 24 volatile organic compounds (VOCs) in water samples is presented. The method allows for the simultaneous quantification of benzene, toluene, ethyl benzene, and xylenes (BTEX), methyl tert-butyl ether (MTBE), tert-butyl alcohol (TBA), as well as a variety of chlorinated methanes, ethanes, propane, enthenes and benzenes. Applying a liquid film polyethylene glycol or a porous layer open tubular (PLOT) divinylbenzene GC capillary column to separate the water from the VOCs, volumes of 1-10 microL aqueous sample are directly injected into the GC. No enrichment or pretreatment steps are required and sample volumes as low as 100 microL are sufficient for accurate quantification. Method detection limits determined in natural groundwater samples were between 0.07 and 2.8 microg/L and instrument detection limits of <5 pg were achieved for 21 out of the 24 evaluated VOCs. DAI-GC/MS offers both good accuracy and precision (relative standard deviations 相似文献   

Simultaneous determination of cyclophosphamide, ifosfamide, doxorubicin, epirubicin and daunorubicin in human urine using high-performance liquid chromatography/electrospray ionization tandem mass spectrometry: bioanalytical method validation

A reversed-phase high-performance liquid chromatography (rp-HPLC) system interfaced with an electrospray ionization (ESI) source coupled to tandem mass spectrometry (MS/MS) was developed and validated for the determination of cyclophosphamide (CP), ifosfamide (IF), daunorubicin (DNR), doxorubicin (DXR), and epirubicin (EPI) in human urine. The analysis of samples containing multiple analytes with a dissimilar range of polarities was carried out using a conventional reversed-phase chromatographic BDS Hypersil C8 column. The analytical run was 15 min. The triple quadrupole mass spectrometer was operated in positive ion mode and multiple reaction monitoring (MRM) was used for drug quantification. The method was validated over a concentration range of 0.2 to 4.0 microg.L(-1) for CP, IF, DXR, EPI and 0.15-2.0 microg.L(-1) for DNR in human urine. The lower limit of quantification (LLOQ) was 0.2 microg.L(-1) for CP, IF, EPI and was set at 0.3 and 0.15 microg.L(-1) for DXR and DNR, respectively. The relative standard deviations (RSD%) were <11.2% for inter- and intra-day precisions. The overall accuracy was also within 114.7% for all analytes at the concentrations of the quality control samples. The potential of ionization suppression resulting from the endogenous biological material on the rp-HPLC/MS/MS method was evaluated and measured. The feasibility of the proposed HPLC/ESI-MS/MS procedure was demonstrated by analyzing urine samples from pharmacy technicians and nurses working in hospitals or personnel employed in drug-manufacturing plants.     

Determination of cefuroxime in human serum or plasma by liquid chromatography with electrospray tandem mass spectrometry

Cefuroxime is a second-generation cephalosporin used against different kinds of bacterial infections. To be able to optimize the dosing it is necessary to characterize the pharmacokinetics of cefuroxime which requires a selective and sensitive analytical method for cefuroxime in plasma or serum. A new rapid liquid chromatography/electrospray tandem mass spectrometry (LC/MS/MS) method, using cefotaxime as internal standard, was developed for analysis of cefuroxime in human serum. The work-up procedure consisted of protein precipitation with acetonitrile/cefotaxime, and after centrifugation the supernatant was dissolved in mobile phase. The sample was injected on a SB-CN column and the detection was performed using tandem mass spectrometry (MS/MS). The limit of quantification was determined to 0.025 microg/mL. The method was linear in the range 0.025-50 microg/mL with a coefficient of correlation >0.999. The limit of quantification and intra-day variability were found to be the same for plasma samples, which indicates that the method is valid for serum as well as plasma samples.     

Optimization of solid phase extraction clean up and validation of quantitative determination of corticosteroids in urine by liquid chromatography-tandem mass spectrometry

A solid phase extraction (SPE) method for extraction and clean up of 9 synthetic corticosteroids was optimized for quantification by reversed-phase high-performance liquid chromatography/negative electrospray ionisation mass spectrometry. Clean up was accomplished using a mixed mode polymeric strong anion exchange SPE column. The final method was validated according to EU regulations for determination of residues of veterinarian drugs in products of animal origin. Initial results showed a large difference in ion suppression between samples of porcine and bovine urine. The aim of optimisation was to design a procedure that minimised this difference while using a single SPE procedure and a fast HPLC method that enabled sufficient separation of the epimers beta- and dexamethasone. To include conjugated corticosteroids in the analysis, the sample was hydrolysed with Helix Pomatia beta-glucuronidase/aryl sulfatase. For the final method, which included fluocinolone acetonid, triamcinolone acetonid, beclomethasone, flumethasone, dexamethasone, betamethasone, 6alpha-methylprednisolone, prednisone and prednisolone, a quantification based on spiked samples carried through the entire analytical procedure was used. For quantification of triamcinolone acetonid an internal standard (triamcinolone acetonid-D6) was used. Relative average recoveries from 96 to 103% were found, except for beclomethasone (113%). Absolute average recoveries were 81-99%. Quantification limits (decision limits, CCalpha) were demonstrated to be not higher than 1 microg L(-1) (3 microg L(-1) for prednisone and prednisolone). The internal reproducibility, determined by triplicates from spiking at three different levels in six analytical series was 7-19% (at 2-4 microg L(-1)) except for prednisone and prednisolone (26-27% at 3-6 microg L(-1)).     

高效液相色谱-质谱法测定比格犬血浆中的艾普拉唑及其药代动力学

运用高效液相色谱-电喷雾质谱(HPLC-ESI-MS)技术,建立了快速、简单、灵敏的比格犬静脉滴注艾普拉唑钠盐后血药浓度的检测方法。血浆样品采用蛋白沉淀法,以丁螺环酮作为内标,色谱柱为Teknokroma Kromasil C18(100 mm×2.1 mm, 5 μm),流动相为水-甲醇-乙腈(69:8:23, v/v/v)(含0.1%的甲酸),流速0.2 mL/min,采用电喷雾(ESI)离子源以正离子方式检测。绘制血药浓度-时间曲线,并采用DAS 2.0计算药代动力学参数。方法学实验结果表明内源性杂质不干扰艾普拉唑和内标的测定,线性范围为5～10000 μg/L (r=0.994),最低定量限为5 μg/L,精密度和准确度均符合生物样品测定的要求。低、中、高3个浓度的绝对回收率在106%左右,基质效应小于142.0%,表明该方法适合比格犬血浆中艾普拉唑浓度的测定及药代动力学研究。比格犬静脉滴注艾普拉唑钠盐3个剂量(0.2 mg/kg、0.8 mg/kg和3.2 mg/kg)后的药-时曲线下面积(AUC(0~∞))分别为(2.4×104±3×103)、(8.8×104±1.6×104)和(5.4×105±8×104) μg/L•min,呈线性药物代谢动力学过程。     

三甲基硅烷衍生化-气相/质谱联用法分析尿中7-氨基硝西泮

 建立了分析尿中硝西泮主要代谢物 7 氨基硝西泮 (7 ANIZ)的三甲基硅烷衍生化 气相 /质谱联用方法。尿样经乙醚 乙酸乙酯 (体积比为 99∶1 )萃取后 ,用N ,O 双 (三甲基硅 )三氟乙酰胺进行衍生化 ,检测衍生物的总离子流。根据 7 ANIZ衍生物质谱中主要特征离子的相对丰度及其质量的保留时间进行定性分析 ;用 7 氨基氯硝西泮做内标 ,根据衍生物基峰离子的质量进行定量分析。本方法中 7 ANIZ的萃取率为 82 8% ,线性范围为 1 0 μg/L～ 50 0 μg/L,检出限为 1 2 μg/L,定量限为 3 5μg/L。     

Sensitive determination of acidic drugs and triclosan in surface and wastewater by ion-pair reverse-phase liquid chromatography/tandem mass spectrometry

A new method is presented for the determination of 12 acidic pharmaceuticals (non-steroidal anti-inflammatory drugs and bezafibrate), including two metabolites from aqueous samples, together with triclosan as a personal care product. Ion-pair liquid chromatography (IP-LC) with electrospray ionisation tandem mass spectrometry (ESI-MS) in the negative ion mode was employed. The ion-pairing agent (tri-n-butylamine) increased the signal intensity for all acidic analytes and detection limits of 6-200 ng/L were obtained by multiple reaction monitoring. This allows analysis of wastewater samples by direct injection into the LC/MS system without the need for a preceding enrichment step. When combined with a solid-phase extraction (SPE) step, limits of quantification between 0.15 and 11 ng/L were obtained from 100-mL sample volumes, which is adequate for most applications. The occurrence of matrix effects was studied and standard addition was required for reliable quantification after SPE from wastewater. The method was finally applied to surface and wastewaters, with analyte concentrations ranging from below the detection limit up to 5.5 microg/L.     

Micellar electrokinetic chromatography for the analysis of cefpirome in microdialysis and plasma samples obtained in vivo from human volunteers

Pharmacokinetics of drugs in the human interstitial space fluid can be monitored by means of microdialysis. However, the small-volume microdialysis samples containing low drug concentrations require a sensitive analytical method. In the present study, micellar electrokinetic chromatography (MEKC) is described for the quantification of cefpirome in human microdialysis and plasma samples. Sample preparation of human plasma samples by ultracentrifugation was suitable for comparison of plasma and microdialysate concentrations. Limits of quantification were 2 microg/mL and 0.3 microg/mL for plasma and microdialysate samples, respectively. The limit of detection (LOD) was estimated at 0.2 microg/mL for the plasma and microdialysate samples. In conclusion, MEKC is a reliable and reproducible technique for measuring cefpirome concentrations in microdialysates as well as centrifuged plasma samples.     

Investigation of the pharmacokinetics of celecoxib by liquid chromatography-mass spectrometry

A new method for the quantification of celecoxib in human plasma based on reversed-phase high-performance liquid chromatography (HPLC) coupled to atmospheric pressure chemical ionization (APCI) mass spectrometry (MS) after liquid-liquid extraction is presented. The method is rapid, sensitive and highly selective. The retention time of celecoxib was 2.3 min. The limit of quantification was 5 microg/L. Rofecoxib was used as internal standard. After validation, the method was used to study the pharmacokinetic profile of celecoxib following administration of a single oral dose (200 mg) in 12 healthy volunteers. Since celecoxib should be metabolized primarily by cytochrome 2C9 (CYP2C9), a poor metabolizer (PM) for this cytochrome P450 enzyme was included in the study. Pharmacokinetic characteristics (mean +/- SD) of extensive metabolizers (EM) were t(max) 2.9+/-1.2h, c(max) 842+/-280 microg/L, AUC(infinity) 6246+/-2147 microg h/L and t(1/2) 7.8+/-2.7h. The area under the curve (AUC(infinity)) for the PM was 12561 microg h/L. However, we found no noticeable increase in half life in the PM (11.5 h) after a single dose of celecoxib.     

Liquid chromatography/electrospray ionization mass spectrometry method for the quantification of valproic acid in human plasma

A simple, sensitive and rapid liquid chromatography/electrospray ionization mass spectrometry (LC/ESI-MS) method was developed and validated for the quantification of valproic acid, an antiepileptic drug, in human plasma using benzoic acid as internal standard (IS). Following solid-phase extraction, the analytes were separated using an isocratic mobile phase on a reversed-phase C18 column and analyzed by MS in the single ion monitoring mode using the respective [M-H]- ions, m/z 143 for valproic acid and m/z 121 for the IS. The assay exhibited a linear dynamic range of 0.5-60 microg/mL for valproic acid in human plasma. The lower limit of quantification was 500 ng/mL with a relative standard deviation of less than 10%. Acceptable precision and accuracy were obtained for concentrations over the standard curve range. The average absolute recoveries of valproic acid and the IS from spiked plasma samples were 96.1+/-4.2 and 95.6+/-2.7%, respectively. A run time of 4.5 min for each sample made it possible to analyze more than 250 human plasma samples per day. The validated method has been successfully used to analyze human plasma samples for application in pharmacokinetic, bioavailability and bioequivalence studies.     

Quantitative determination of paroxetine and its 4-hydroxy-3-methoxy metabolite in plasma by high-performance liquid chromatography/electrospray ion trap mass spectrometry: application to pharmacokinetic studies

A high-performance liquid chromatography (HPLC) method with tandem mass spectrometric detection is described for the determination of paroxetine, an antidepressant drug, and its metabolite (3S,4R)-4-(4-fluorophenyl)-3-(4-hydroxy-3-methoxyphenoxymethyl)piperidine (HM paroxetine) in human plasma. Plasma samples were hydrolysed with hydrochloric acid and then analytes were extracted with ethyl acetate at alkaline pH. Extracts were analysed by HPLC coupled to an atmospheric pressure ionisation-electrospray (ESI) interface and an ion trap mass spectrometer. Chromatography was performed on a reversed-phase column using acetonitrile/0.02% formic acid (66:34, v/v) as a mobile phase. The mass spectrometer was operated in the multiple reaction monitoring mode. The method was validated over concentration ranges of 0.75-100 microg/L and 5-100 microg/L for paroxetine and HM paroxetine, respectively. Mean recoveries of 77% for paroxetine and 76% for HM paroxetine were found, with precision always better than 15%. The limits of detection and quantification were 0.20 and 0.70 microg/L for paroxetine, and 0.70 and 2.20 microg/L for its metabolite. The method was applied to the analysis of plasma samples obtained from nine healthy male volunteers administered with a single oral dose of 20 mg paroxetine. After the 20-mg dose, the mean peak plasma concentration was 8.60 microg/L for paroxetine and 92.40 microg/L for HM paroxetine showing a tenfold ratio between the metabolite and the parent drug along the entire time-concentration curve.     

Development of water-phase derivatization followed by solid-phase microextraction and gas chromatography/mass spectrometry for fast determination of valproic acid in human plasma

In this study, a simple, rapid, and sensitive method was developed and validated for the quantification of valproic acid (VPA), an antiepileptic drug, in human plasma, which was based on water-phase derivatization followed by headspace solid-phase microextraction (HS-SPME) and gas chromatography/mass spectrometry (GC/MS). In the proposed method, VPA in plasma was rapidly derivatized with a mixture of isobutyl chloroformate, ethanol and pyridine under mild conditions (room temperature, aqueous medium), and the VPA ethyl ester formed was headspace-extracted and simultaneously concentrated using the SPME technique. Finally, the analyte extracted on SPME fiber was analyzed by GC/MS. The experimental parameters and method validations were studied. The optimal conditions were obtained: PDMS fiber, stirring rate of 1100 rpm, sample temperature of 80 degrees C, extraction time of 20 min, NaCl concentration of 30%. The proposed method had a limit of quantification (0.3 microg/mL), good recovery (89-97%) and precision (RSD value less than 10%). Because the proposed method combined a rapid water-phase derivatization with a fast, simple and solvent-free sample extraction and concentration technique of SPME, the sample preparation time was less than 25 min. This much shortens the whole analysis time of VPA in plasma. The validated method has been successfully used to analyze VPA in human plasma samples for application in pharmacokinetic studies. All these results show that water-phase derivatization followed by HS-SPME and GC/MS is an alternative and powerful method for fast determination of VPA in biological fluids.     

Simultaneous determination of paracetamol and dextropropoxyphene in human plasma by liquid chromatography/tandem mass spectrometry: application to clinical bioequivalence studies

A liquid chromatography/mass spectrometry method for simultaneous determination of paracetamol and dextropropoxyphene in human plasma is described. Paracetamol and dextropropoxyphene, together with their internal standards (tolbutamide and pyrroliphene), were extracted from 0.5 mL of plasma using solid-phase extraction. The chromatography was performed using a Thermo Hypersil APS-2 Amino column (250 mm x 4.6 mm, 5 microm) with a mobile phase consisting of acetonitrile and 0.4% glacial acetic acid in water (20:80). The total run time was 6 min for each sample. The triple-quadrupole mass spectrometer was operated in both positive (for detection of dextropropoxyphene and its IS pyrroliphene) and negative (for detection of paracetamol and its IS tolbutamide) modes using a polarity-switching technique. Multiple reaction monitoring was used for quantification. The method was linear over the concentration range of 0.1-20 microg/mL for paracetamol and 0.5-80 ng/mL for dextropropoxyphene. The intra- and inter-day precision were less than 10%, and the accuracy ranged from 92.2-110.9%. The lower limits of quantification were 0.1 microg/mL for paracetamol and 0.5 ng/mL for dextropropoxyphene. The present method provides a robust, fast and sensitive analytical tool for both paracetamol and dextropropoxyphene, and has been successfully applied to a clinical bioequivalence study in 14 subjects.     

Determination of Se4+ in drinkable water by solid-phase microextraction and gas chromatography/mass spectrometry

A method was developed for the selective determination of Se4+ in drinkable water by solid-phase microextraction (SPME) and gas chromatography/mass spectrometry (GC/MS). Se4+ was selectively derivatized to ethane, 1,1'-selenobis by reaction with sodium tetraethylborate, extracted by the SPME fiber, and determined by GC/MS. Both headspace (HS)-SPME and direct SPME were studied. The method requires only a few milliliters of sample and 20 min for completion. At 2.0 microg/L concentration, the relative standard deviation was 10.1% for HS-SPME and 9.1% for direct SPME. For HS-SPME, the theoretical detection limit was 81 ng/L and 166 ng/L for direct SPME. The recovery rate was 95%. The method was used to determine Se4+ in 10 tap water samples.     

Rapid gas chromatography/mass spectrometry quinine determination in plasma after automated solid-phase extraction

The combined use of an automatic solid-phase extraction (SPE) apparatus with Oasis MCX cartridges and gas chromatography/mass spectrometry (GC/MS) to rapidly quantify quinine in biological samples with cyproheptadine as the internal standard is described. The selected ion monitoring mode, with the quantification ions m/z 136 and 287 (qualifier ions: m/z 261, 381 and 215, 96), allows the estimation of quinine levels, respectively. Separation was completed within 12.7 min. Excellent linearity was found up to 10 000 microg/L of plasma. The limit of detection (LOD) was 12.2 microg/L and the limit of quantification (LOQ) was 40.6 microg/L. High reproducibility (intra-assay CV range 1.9-4.3%, inter-assay CV range 2.2-11.3%) and accuracy values (intra-assay range 83.2-103.7%, inter-assay range 86.8-103.7%) were obtained. Recoveries were concentration-independent (97.2% and 89.8% for 4000 and 10 000 microg/L, respectively). This sensitive, simple assay for quinine in various matrices meets the current requirements for bioanalytical assays and may be used to monitor quinine levels in patients developing severe malaria with acute renal failure during hemofiltration. The optimal quinine dose in this situation is not really established and to improve clinical care, quinine concentrations might be explored to improve efficacy and minimise potential toxicity.     

An automated analyzer for vancomycin in plasma samples by column-switching high-performance liquid chromatography with UV detection

An automated analyzer for vancomycin in rat plasma by column-switching high-performance liquid chromatography (HPLC) with UV detection was developed. The method includes in-line extraction of vancomycin by ion-exchange cartridge column and a separation on a reversed-phase column with UV detection at 215 nm. Plasma samples were diluted by mobile phase solution and directly injected to HPLC. Vancomycin was quantitatively recovered from rat plasma samples. The separation was completed within 15 min. The calibration curve was linear over the range from 0.5 to 100 microg/mL with the detection and quantification limits of 0.5 microg/mL (2.5 ng on column; signal-to-noise ratio = 3). The values of precision in intra- and inter-day assays (n = 3) were less than 1.92 and 3.69%, respectively. This method does not require time-consuming pre-treatment and is suitable for the routine assay of plasma samples.     

超高效液相色谱-串联质谱法测定大鼠血浆中的磷酸西他列汀

建立了大鼠血浆中磷酸西他列汀含量检测的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。以大鼠空白血浆为基质,通过添加标准品的方法配制含磷酸西他列汀和内标物氟西汀的样品,选用甲醇为沉淀剂,经离心除去血浆中的蛋白质,上清液用于目标物的检测。采用Thermo Hypersil Gold C18柱(50 mm×2.1 mm, 1.9 μm)为分析柱,Phenomenex Security Guard C18(4 mm×3.0 mm)为预柱,以乙腈和0.05%(v/v)甲酸水溶液为流动相进行梯度洗脱,流速为200 μL/min, 5 min内实现了快速分离。采用电喷雾正离子(ESI+)模式电离,选择反应监测(SRM)模式检测,确定了磷酸西他列汀和氟西汀的监测离子对分别为m/z 408.0→235.0和m/z 310.0→148.0,用基质匹配标准溶液法进行定量。结果表明: 大鼠血浆中磷酸西他列汀的质量浓度在1～1000 μg/L范围内时线性关系良好(r=0.9991),检出限(信噪比为3)为0.2 μg/L;其平均回收率为85%～115%;日内及日间的相对标准偏差(RSDs)均小于15%,满足生物样品检测的要求。将该方法初步用于大鼠静脉注射后的血浆样品中磷酸西他列汀的检测。该方法快速、灵敏度高、操作简便、重现性好,能够用于磷酸西他列汀药代动力学等方面的研究。     

超高效液相色谱-串联质谱法测定兔血浆中的丝裂霉素C

建立了采用超高效液相色谱-串联质谱测定兔血浆中丝裂霉素C的方法。以兔空白血浆为基质,通过添加标准溶液的方法配制含丝裂霉素C和内标物曲安奈德的样品,选用乙酸乙酯为提取溶剂,液-液萃取法处理血浆样品。采用Hypersil Gold C18分析柱(50 mm×2.1 mm, 1.9 μm),流动相为甲醇-0.1%甲酸水溶液(90:10, v/v),等度洗脱,流速0.2 mL/min,柱温35 ℃,在3 min内实现了快速分离。采用电喷雾正离子(ESI+)模式电离,选择反应监测(SRM)模式检测,以曲安奈德作为内标物进行定量。用于监测的定量离子对分别为丝裂霉素C m/z 335.2→242.2和曲安奈德m/z 435.2→397.3/415.2,用基质匹配标准溶液法进行定量。结果表明: 兔血浆中丝裂霉素C的质量浓度在1～1000 μg/L范围内线性关系良好(r=0.9978,权重系数(weighting): 1/x2);血浆中丝裂霉素C的检出限(信噪比为3)为0.2 μg/L;其平均回收率为85%～ 115%;日内及日间的相对标准偏差(RSDs)均小于15%,满足生物样品检测的要求。该方法可用于兔气管外壁给药后的血浆样品中丝裂霉素C的检测。本方法选择性强、灵敏度高、操作简便快速、重现性好,适用于丝裂霉素C药代动力学等方面的研究。