Detection of glutathione conjugates derived from 4-ipomeanol metabolism in bile of rats by liquid chromatography-tandem mass spectrometry.

Earlier studies postulated that bioactivation of 4-ipomeanol by cytochrome P450 enzymes may occur through oxidation of its furan ring, following a mechanism similar to the bioactivation of other furan-containing compounds. This would lead to the formation of furan epoxides and alpha,beta-unsaturated di-aldehyde-reactive metabolites that can conjugate with glutathione. These metabolites are thought to be responsible for the cytotoxic and anticancer properties of 4-ipomeanol. We hypothesized that if 4-ipomeanol is metabolized following this pathway, its glutathione conjugates would be isobaric (molecular ion mass = 492 Da) and would be excreted in bile. To investigate this hypothesis, we analyzed by liquid chromatography-tandem mass spectrometry the bile of rats administered d0/d6 4-ipomeanol (1:1 ratio) intravenously. Hexadeuterated 4-ipomeanol had all deuterium atoms incorporated on its aliphatic chain. Multiple reaction monitoring scans of bile for the mass transition: MH+/(MH - 129)+, which is characteristic of glutathione conjugates, detected four glutathione conjugates. The observation of the isotope cluster (M + 1)+ (d0)/(MH + 6)+ (d6) in a 1:1 molar ratio confirmed that these conjugates were derived from 4-ipomeanol. Retention of the six deuterium atoms in the glutathione conjugates detected, (MH + 6)+, indicates that the bioactivation of 4-ipomeanol took place on the furan ring moiety. Rat hepatic microsomal incubations provided additional evidence. From this study, the mass of the reactive metabolites of 4-ipomeanol can be inferred. The inferred mass (186 Da) matches the mass postulated. A pathway of 4-ipomeanol bioactivation is proposed here. This work represents one step forward to understanding the mechanism of bioactivation of 4-ipomeanol.     

Detection of levamisole exposure in cocaine users by liquid chromatography-tandem mass spectrometry

Levamisole, a veterinary antihelminthic, was recently recognized as an adulterant in cocaine and is known to cause severe adverse reactions in some cocaine users. Because of the health concerns involving levamisole-adulterated cocaine, we developed a liquid chromatography-tandem mass spectrometry (LC-MS-MS) method for the detection of levamisole in urine. This method was used to determine the prevalence of levamisole in cocaine-positive patient samples. All cocaine-positive urine samples that were sent to the San Francisco General Hospital Clinical Laboratory were tested for levamisole for one month. For LC, an Agilent 1200 series was used with a C(18) column and a gradient of mobile phase A (0.05% formic acid) and B (acetonitrile/methanol). Detection was carried out with an Applied Biosystems QTRAP(?) LC-MS-MS. The levamisole LC-MS-MS method was linear over the range of 5-2500 ng/mL (r > 0.996). Interassay and intraassay CVs were < 6%. The lower limit of detection for levamisole was 0.5 ng/mL. Out of 949 total urine drug screens, 20% were positive for benzoylecgonine, and of those, 88% were positive for levamisole. The high prevalence of levamisole-adulterated cocaine and potential toxicity in cocaine users is a serious public health concern. These findings validate the utility of an LC-MS-MS method for the detection of levamisole.     

Drug screening of hair by liquid chromatography-tandem mass spectrometry

Hair has become an important matrix for drug analysis, complementary to blood and urine as a matrix. A prolonged detection window makes hair analysis suitable for the detection of exposure to illegal and medicinal drugs for periods up to 12 months. In the present study, a liquid chromatography-tandem mass spectrometry (LC-MS-MS) method for drug screening in hair was developed and validated. To 20 mg of hair, 0.45 mL of acetonitrile/25 mM formic acid (5:95 v/v) and 50 microL of deuterated internal standards were added, and the sample was incubated in a water bath at 37 degrees C for 18 h. LC separation was achieved with a Zorbax SB-Phenyl column (2.1 x 100 mm, 3.5-microm particle). Mass detection was performed by positive ion mode electrospray LC-MS-MS and included the following drugs/metabolites: nicotine, cotinine, morphine, 6-monoacetylmorphine, codeine, amphetamine, methamphetamine, 3,4-methylenedioxymeth-amphetamine, cocaine, benzoylecgonine, 7-aminonitrazepam, 7-aminoclonazepam, 7-aminoflunitrazepam, oxazepam, diazepam, alprazolam, zopiclone, zolpidem, carisoprodol, meprobamate, buprenorphine, and methadone. Within- and between-assay relative standard deviations varied from 2.0% to 12% and 2.7% to 15%, respectively. The accuracies were in the range of -24% to 16%, and recoveries ranged from 25% to 100%. The LC-MS-MS method proved to be simple and robust for the determination of drugs in hair. It has been used for authentic samples in our laboratory in the past year.     

液质联用法测定人血浆中沙格雷酯的浓度

目的建立人血浆中沙格雷酯质量浓度的液相色谱-串联质谱(LC-MS/MS)测定方法。方法色谱柱为Elipse XDB-C18柱,流动相为乙腈-0.01 mol·L-1醋酸铵(体积比为65∶35),血浆样品经乙腈沉淀蛋白处理,以选择反应监测(selected reaction monitoring,SRM)扫描方式检测,测定健康男性受试者经口给予盐酸沙格雷酯后血浆中沙格雷酯的质量浓度。结果沙格雷酯线性为5.0¹ 000μg·L-1,定量下限为5.0μg·L-1。日内、日间精密度(Relative Standard Deviation,RSD)均不大于9.0%,准确度(Relative Error,RE)为-6.5%1 000μg·L-1,定量下限为5.0μg·L-1。日内、日间精密度(Relative Standard Deviation,RSD)均不大于9.0%,准确度(Relative Error,RE)为-6.5%².6%。沙格雷酯在健康男性血浆中主要药动学参数tmax为(0.49±0.21)h,ρmax为(725±264)μg·L-1,t1/2为(0.58±0.21)h,AUC0-t为(534±111)μg·h·L-1,AUC0-∞为(540±111)μg·h·L-1。结论该方法适用于沙格雷酯在健康人体内药动学的研究。     

高效液相色谱-串联质谱法测定人血清中替加环素的浓度

目的：建立人血清中替加环素浓度的高效液相色谱-串联质谱法（HPLC-MS/MS）测定方法。方法：以[叔丁基-d9]替加环素为内标,将待测血清样品经氢氧化钠碱化后,加乙酸乙酯-二氯甲烷（4∶1,V/V）提取,上清液经真空干燥,得到的残渣经流动相复溶后进样。进样液经Agilent Eclipse plus C₈（4.6 mm×100 mm,5 μm）色谱柱分离,甲醇-水（30∶70,V/V,含0.005 mol·L^-1甲酸铵和0.25%甲酸）为流动相,流速0.5 mL·min^-1,进行洗脱,采用电喷雾电离源（ESI）,以多反应监测（MRM）方式进行正离子检测。用于定量分析的离子分别为替加环素m/z586.4→513.3和[叔丁基-d9]替加环素m/z595.4→514.3。结果：血清中替加环素的浓度与峰面积比在10~2 000 ng·mL^-1范围内线性关系良好,定量下限为10 ng·mL^-1,提取回收率大于70.04%,日内日间精密度小于4.54%。结论：该法简单、灵敏、快速,分离效果良好,可用于人体血药浓度测定和PK/PD研究。     

Direct analysis of opiates in urine by liquid chromatography-tandem mass spectrometry

A method for the direct analysis of 10 opiate compounds in urine was developed using liquid chromatography-mass spectrometry-mass spectrometry (LC-MS-MS) with electrospray ionization interface (ESI). Opiates included were morphine-3-P-glucuronide, morphine-6--glucuronide, morphine, oxymorphone, hydromorphone, norcodeine, codeine, oxycodone, 6-monoacetylmorphine (6MAM), and hydrocodone. Urine samples were prepared by centrifugation to remove large particles and direct injection into the LC-MS-MS. Separation and detection of all compounds was accomplished within 6 min. Linearity was established for all opiates except 6MAM from 50 ng/mL to 10,000 ng/mL; 6MAM from 0.25 ng/mL to 50 ng/mL with all correlation coefficients (r) > 0.99. Interrun precision (%CV) ranged from 1.1% to 16.7%, and intrarun precision ranged from 1.3% to 16.3%. Accuracy (% bias) ranged from -7.3% to 13.6% and -8.5% to 11.8 for inter- and intrarun, respectively. Eighty-nine urine samples previously analyzed by gas chromatography-MS were re-analyzed by the LC-MS-MS method. The qualitative results found an 88% agreement for negative samples between the two methods and 94% for positive samples. The LC-MS-MS method identified 19 samples with additional opiates in the positive samples. Overall, the direct injection LC-MS-MS method performed well and permitted the rapid analysis of urine samples for several opiates simultaneously without extensive sample preparation.     

液相色谱-串联质谱法测定人血浆中的利培酮

利培酮为苯并异噁唑类化合物,通过阻断5-HT2受体和多巴胺D2受体发挥抗精神病作用.同其他抗精神病药物相比,利培酮所引起的椎体外系副作用更少,药效更为明显 .     

液相色谱-质谱-质谱联用法测定猕猴血浆中阿德福韦液相色谱-质谱-质谱联用法测定猕猴血浆中阿德福韦

目的 建立测定猕猴血浆中阿德福韦(adefovir)的液相色谱-质谱-质谱联用法。方法 取血浆样品0.25 mL经甲醇沉淀蛋白后,以甲醇-水-甲酸(20∶80∶1)为流动相,用Diamonsil C₁₈柱分离,通过电喷雾离子化四极杆串联质谱,以选择离子反应监测方式进行检测。用于定量分析的离子反应分别为m/z 274→m/z 162(阿德福韦)和m/z 288→m/z 176［内标,9-(3-膦酸甲氧基丙基)腺嘌呤］。结果阿德福韦线性范围为0.02～4.00 mg·L^-1,最低定量限为20 μg·L^-1,日内、日间精密度(RSD)小于5.8%,准确度(RE)在±4.5%范围内。在临床前药代动力学研究中,应用此法测试了3只猕猴po给予阿德福韦地匹福酯(adefovir dipivoxil)后血浆中阿德福韦的浓度。结论该法操作简便,准确,适用于临床前药代动力学研究。     

液相色谱-串联质谱法测定人血浆中奥洛他定的浓度

目的建立人血浆中奥洛他定浓度测定的液相色谱-串联质谱（LC—MS／MS）定量方法。方法以地氯雷他定为内标,血浆样品经蛋白沉淀处理后,在0．2mL·min^-1的流速下以乙腈-甲醇-0．1％甲酸水溶液（25：5：70,V／V／V）为流动相进行等度洗脱,采用CAPCELLPAKC18柱（50mm×2．1mm,3．5μm）分离。样品经电喷雾离子源（ESI）正离子化后,通过三重四极杆串联质谱仪,采用多反应离子检测方式测定奥洛他定（m／z338．2／165．2）和内标地氯雷他定（m／z311．1／259．1）的浓度。结果奥洛他定质量浓度在1～200μg·L^-1内线性良好,定量下限为1μg·L^-1,方法回收率为85％-115％,批内、批间RSD均〈10％。结论本方法专属性强、灵敏度高,操作简便、快速,符合生物样品分析要求,适用于临床药动学研究。     

LC-MS/MS法测定人体血浆中谷氨酰胺的含量

目的建立测定人血浆中谷氨酰胺浓度的液相色谱串联质谱法(LC-MS/MS)。方法血浆样品用质量分数为10%的三氯乙酸沉蛋白,色谱柱:Inertsil-CN柱,流动相:5 mmol·L~(-1)醋酸铵(含体积分数为0.1%的甲酸)-甲醇-乙腈(体积比为70∶15∶15),流速:750μL·min~(-1),质谱:采用多反应检测模式,API2000电喷雾离子源。结果谷氨酰胺的线性为12~384 mg·L~(-1),定量下限为12 mg·L-1,日间日内精密度(relative standard deviation,RSD)均不大于15%。健康男性受试者单剂量口服谷氨酰胺颗粒5 g后的主要药动学参数为:tmax为(0.77±0.13)h,ρmax为(75.3±29.0)mg·L~(-1),t_(1/2)为(1.83±1.93)h,采用梯形法计算,AUC_(0-t)为(109.2±40.1)mg·h·L~(-1),AUC_(0-∞)为(114.0±40.4)mg·h·L~(-1)。结论该法适合于谷氨酰胺颗粒的人体药动学研究。     

液相色谱-串联质谱法研究YL-0919在小鼠体内的药动学(英文)

目的建立测定小鼠血浆中YL-0919的液相色谱-串联质谱(LC-MS/MS)法,并研究其在小鼠体内的药动学。方法小鼠分别单剂量口服YL-0919不同剂量(2,6,18 mg·kg~(-1))后,于不同时间点采血,LC-MS/MS法测定血浆中YL-0919的浓度,并计算药动学参数。结果 YL-0919在2～2 000μg·L~(-1)范围内线性关系良好,最低定量限为2μg·L~(-1),提取回收率大于80%,日内、日间RSD均小于11%。小鼠分别单剂量口服YL-0919 2、6、18 mg·kg~(-1)后,吸收和消除迅速,t_(max)均为0.083 h,MRT为0.35～0.44 h,给药6 h后血药浓度低于定量下限;ρ_(max)分别为35.32、177.31和1 358.37μg·L~(-1);AUC_(0-6 h)分别为12.51、68.99和585.78μg·h·L~(-1);AUC_(0-∞)分别为16.29、69.99和594.97μg·h·L~(-1);随给药剂量增加,ρ_(max)和AUC的增大倍数高于剂量的增大倍数。结论本法简便、灵敏、准确,适用于YL-0919在小鼠体内的药动学研究。     

液质联用法测定人血浆中米格列奈的浓度

目的建立LC-MS/MS法测定人血浆中米格列奈的浓度,并研究其在健康男性受试者体内的药动学。方法血浆经液-液萃取。色谱柱:Agilent TC-C18柱,流动相:乙腈-水-甲酸(体积比为70.0∶30.0∶0.3),质谱检测采用多反应监测模式(multiple reaction monitoring,MRM),电喷雾离子源,分析时间:2.0 min。结果米格列奈线性为5.0～4 000.0μg.L-1,定量下限为5.0μg.L-1。日内、日间精密度(relative standard deviation,RSD)均不大于10.5%,准确度(relative error,RE)为-0.8%～-2.0%。健康男性受试者口服含米格列奈10 mg的受试制剂(规格:10 mg/片)和参比制剂(规格:5 mg/片)后主要药动学参数为:tmax分别为(0.375±0.079)和(0.396±0.166)h,ρmax分别为(887±292)和(902±298)μg.L-1,t1/2分别为(1.37±0.45)和(1.49±0.57)h,AUC0-t分别为(1047±379)和(1 067±430)μg.h.L-1,AUC0-∞分别为(1 070±394)和(1 092±433)μg.h.L-1。结论该法适用于米格列奈的药动学及生物等效性研究。     

HPLC-MS-MS法测定人血浆中托吡酯的浓度

目的:建立测定人血浆中托吡酯浓度的HPLC-MS-MS方法。方法:采用液液萃取法,以甲基叔丁基醚为提取溶剂;HPLC采用Hypersil ODS C18色谱柱(150 mm×4.6 mm,5μm),流动相为5 mmol·L-1醋酸铵溶液-甲醇(25∶75),流速0.5 mL·min-1;质谱采用ESI源,负离子检测模式,定量分析离子为托吡酯m/z338.1[M-H]-→78.0,双氯芬酸钠m/z294.1[M-H]-→249.7。结果:人血浆中托吡酯的标准曲线范围为10.00~3 600.00 ng.mL-1(n=7),r>0.999;日内和日间精密度均小于8.9%;提取回收率(低、中、高)分别为(75.5±3.1)%,(77.0±1.6)%和(72.8±1.5)%,内标提取回收率为(76.1±3.5)%;基质效应(低、中、高)分别为(99.2±5.6)%,(98.9±4.2)%和(99.4±3.8)%,内标基质效应为(100.4±1.3)%。结论:该方法灵敏、快速、专属性强,可用于人血浆中托吡酯浓度的测定。     

液相色谱-串联质谱法测定人血浆中罗格列酮

目的:建立测定人血浆中罗格列酮的液相色谱-质谱-质谱联用法,并用于临床药动学研究。方法: 血浆样品经液-液萃取后,以乙腈-水-甲酸(90:10:0．5)为流动相,采用Zorbax SB—C18柱分离,通过电喷雾离子化四极杆串联质谱,以选择反应监测(SRM)方式进行检测。用于定量分析的离子反应分别为m／z 358→ 135(罗格列酮)和m／z 256→167(内标苯海拉明)。结果:标准曲线线性范围为0．50～1 000μg·L-1,定量下限为0．50μg·L-1,日内、日间精密度(RSD)均小于7．4％。应用此法测试了20名男性健康受试者口服酒石酸罗格列酮片(相当于罗格列酮4 mg)后血浆中罗格列酮的浓度。结论:该法灵敏、快速、准确,操作简便、线性范围宽,适用于罗格列酮的临床药动学研究。     

Determination of corticosteroids in tissue samples by liquid chromatography-tandem mass spectrometry

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for determination of corticosterone and 11-dehydrocorticosterone (11-DHC) levels in KKA(y) mouse liver and adipose tissue, and hydrocortisone and cortisone levels in human adipose tissue has been developed. The corticosteroids were extracted from liver tissue with methanol/water and ethyl acetate for adipose tissue samples. Corticosterone and 11-DHC were separated with a methanol gradient and hydrocortisone and cortisone with an acetonitrile gradient containing trifluoroacetic acid on a reversed-phase column within 15 min. The corticosteroids were detected after electrospray ionization in positive mode with multiple reaction monitoring (MRM). The limits of quantification (LOQ) were estimated to be 15 nmol/kg liver and 1.6 nmol/kg adipose tissue for corticosterone and 5.4 nmol/kg liver and 0.92 nmol/kg adipose tissue for 11-DHC. The LOQ was estimated to be 0.2 nmol/kg adipose tissue for hydrocortisone and 0.4 nmol/kg adipose tissue for cortisone. The limits of detection (LOD) at 3 times S/N were estimated to be 0.07 nmol/kg adipose tissue for hydrocortisone 0.1 nmol/kg adipose tissue for cortisone. The variation of endogenous levels in KKA(y) mouse from different animals (CV%) was high with mean liver tissue levels of 117+/-25 (S.D.)nmol/kg for corticosterone and 62+/-19 (S.D.)nmol/kg for 11-DHC (n=5) and adipose tissue levels of 39+/-20 (S.D.)nmol/kg for corticosterone and 2.4+/-0.9 (S.D.)nmol/kg for 11-DHC (n=9). Endogenous levels in human biopsy samples from adipose tissue were 12+/-7.0 (S.D.)nmol/kg for hydrocortisone and 3.0+/-1.6 (S.D.)nmol/kg for cortisone (n=16). The new LC-MS/MS methods showed sufficient sensitivity and selectivity for determination of endogenous levels of corticosteroids in both KKA(y) mouse liver and adipose tissue samples and human adipose tissue samples. The selectivity of the methods was verified by analysis of two different productions from each analyte.     

Detection and quantitation of benzo[a]pyrene-derived DNA adducts in mouse liver by liquid chromatography-tandem mass spectrometry: comparison with 32P-postlabeling

The polycyclic aromatic hydrocarbon, benzo[a]pyrene (B[a]P) is a proven animal carcinogen that is potentially carcinogenic to humans. B[a]P is an ubiquitous environmental pollutant and is also present in tobacco smoke, coal tar, automobile exhaust emissions, and charred food. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method using electrospray ionization and selected reaction monitoring (SRM) has been developed for the detection of 10-(deoxyguanosin-N(2)-yl)-7,8,9-trihydroxy-7,8,9,10-tetrahydrobenzo[a]pyrene (B[a]PDE-N(2)dG) adducts formed in DNA following the metabolic activation of B[a]P to benzo[a]pyrene-7,8-dihydrodiol-9,10-epoxide (B[a]PDE). The method involves enzymatic digestion of the DNA sample to 2'-deoxynucleosides following the addition of a stable isotope internal standard, [(15)N(5)]B[a]PDE-N(2)dG, and then solid phase extraction to remove unmodified 2'-deoxynucleosides prior to analysis by LC-MS/MS SRM. The limit of detection of the method was 10 fmol (approximately 3 B[a]PDE-N(2)dG adducts per 10(8) 2'-deoxynucleosides) using 100 microg of calf thymus DNA as the matrix. Calf thymus DNA reacted with B[a]PDE in vitro and mouse liver DNA samples at different time points following dosing intraperitoneally with 50, 100, and 200 mg/kg B[a]P was analyzed. Three stereoisomers of the B[a]PDE-N(2)dG adduct were detected following the reaction of calf thymus DNA with B[a]PDE in vitro. The levels of B[a]PDE-N(2)dG DNA adducts in the mice livers were found to increase in a dose-dependent manner with adducts reaching maximal levels at 1-3 days and then gradually decreasing over time but still detectable after 28 days. A very good correlation (r = 0.962, p < 0.001) was observed between the results obtained for the mouse liver DNA samples using LC-MS/MS SRM as compared to those obtained using a (32)P-postlabeling method. However, the levels of adducts observed following (32)P-postlabeling using butanol enrichment were approximately 3.7-fold lower. The LC-MS/MS method allowed the more precise quantitation of DNA adduct levels that were structurally characterized, in addition to a reduction in the time taken to perform the analysis when compared with the (32)P-postlabeling method.     

Drug screening of whole blood by ultra-performance liquid chromatography-tandem mass spectrometry

An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) method for screening of drugs in whole blood has been developed and validated. Samples were prepared by supported liquid-liquid extraction on ChemElute(?) columns with ethyl acetate/heptane (4:1). LC separation was achieved with an Acquity HSS T3-column (2.1 100 mm, 1.8-μm particle). Mass detection was performed by positive ion mode electrospray MS-MS and included the following drugs/metabolites: morphine, codeine, ethyl morphine, oxycodone, buprenorphine, methadone, cocaine, methylphenidate, amphetamine, methamphetamine, 3,4-methylenedioxymethamphetamine (MDMA), Δ(9)-tetrahydrocannabinol (THC), fentanyl, alprazolam, bromazepam, clonazepam, diazepam, nordiazepam, 3-OH-diazepam, fenazepam, flunitrazepam, lorazepam, nitrazepam, oxazepam, zopiclone, zolpidem, carisoprodol, and meprobamate. The cycle time was 9 min, and within- and between-day relative coefficients of variation varied from 1% to 33% and 2% to 58%, respectively. Extraction recoveries from whole blood were > 50% except for morphine and THC. The limit of quantitation was 0.1 to 521 ng/mL, depending on the drug.     

LC-MS/MS法测定人血浆中麦考酚酸的浓度

目的建立液相色谱-串联质谱(LC-MS/MS)法测定健康人血浆中麦考酚酸浓度的方法,并对受试制剂与参比制剂的生物等效性进行评价。方法20名健康受试者单剂量口服麦考酚吗乙酯胶囊,以兰索拉唑砜为内标,血浆样品经蛋白沉淀处理后,采用CAPCELL PAK C_(18)(50 mm×2.1 mm,3.5μm,No:AKIE01045)分离。样品经电喷雾离子源(ESI)离子化后,通过三级四极杆串联质谱仪,采用多反应离子检测方式测定麦考酚酸(m/z 319.1/191.1)和内标兰索拉唑砜(m/z 384.0/180.0)的浓度,计算主要药动学参数及相对生物利用度。结果麦考酚酸在0.1～20mg·L~(-1)内线性良好,定量下限为0.1 mg·L~(-1)。方法的相对回收率在85%～115%之间,批内、批间RSD均<15%。受试制剂与参比制剂的t_(1/2)分别为(12.45±5.30)、(14.26±7.47)h,t_(max)分别为(0.74±0.36)、(0.75±0.58)h,ρ_(max)缸分别为(10.29±3.29)、(11.43±4.83)mg·L~(-1)。结论建立的LC-MS/MS法专属性强、灵敏度高,操作简便、快速。受试制剂与参比制剂生物等效。     

液相色谱-串联质谱法测定头发中11种阿片类生物碱

建立头发中海洛因、吗啡、单乙酰吗啡等11种阿片类生物碱的液相色谱-串联质谱测定方法,并考察海洛因滥用者头发中阿片类组分的存在情况。头发经冷冻研磨后加入硼酸缓冲液超声30 min,用氯仿-异丙醇(9∶1)提取。用Allure PFP丙基柱,以乙腈-乙酸铵(0.1%甲酸)梯度洗脱分离,采用二级质谱多反应监测模式(MRM)检测11种阿片类生物碱。头发中海洛因、吗啡、单乙酰吗啡等11种阿片类生物碱在对应质量浓度范围内线性良好(r>0.996 0);检测限(LOD)均小于0.05 ng.mg-1;回收率范围为47.2%～110%;日内精密度和日间精密度均小于14%。21例海洛因滥用者头发中均检出了海洛因、单乙酰吗啡、吗啡、可待因、乙酰可待因、氢可酮等主要组分。所建方法灵敏度高、选择性好,适用于同时分析头发中海洛因等11种阿片类生物碱组分,可有效鉴别海洛因滥用与阿片类药物或食品的摄取。     

牡丹皮化学成分的液相色谱-飞行时间串联质谱分析

目的分析牡丹皮中的化学成分。方法应用优化的高效液相色谱-质谱联用方法对牡丹皮供试品进行分析。结果较好地分离了单萜苷、鞣质和酚酮类等38种化学成分。在负离子检测模式下，由电喷雾质谱得到各成分的准分子离子峰，再根据串联飞行时间质谱获得进一步的结构信息，推测出其中38种主要成分的可能结构。并对牡丹皮中主要化学成分的质谱裂解规律进行了分析。结论本方法能快速检测牡丹皮的化学成分。