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高效液相色谱-质谱联用技术原理与应用

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高效液相色谱-质谱联用技术原理与应用高效液相色谱-质谱联用技术原理与应用什么是液质联用(LC/MS)LC:液湘色谱仪一种能够把液体混合物中的不同组分根据在色谱柱中保留时间不同进行分离,检测及收集的仪器MS:MassSpectrometer质谱仪一种能够把分子转化生成带电离子,并在气态中根据质荷比(m/z:m质量z分子所带电荷数)的不同把离子进行分离并进行检测的仪器.质谱分析过程:样品通过进样系统进入离子源,由于结构性质不同而电离为各种不同质荷比(m/z)的分子离子和碎片离子,而后,带有样品信息的离子碎片被加速进入质量分析器,不同的离子在质量分析...

高效液相色谱-质谱联用技术原理与应用
高效液相色谱-质谱联用技术原理与应用什么是液质联用(LC/MS)LC:液湘色谱仪一种能够把液体混合物中的不同组分根据在色谱柱中保留时间不同进行分离,检测及收集的仪器MS:MassSpectrometer质谱仪一种能够把分子转化生成带电离子,并在气态中根据质荷比(m/z:m质量z分子所带电荷数)的不同把离子进行分离并进行检测的仪器.质谱分析过程:样品通过进样系统进入离子源,由于结构性质不同而电离为各种不同质荷比(m/z)的分子离子和碎片离子,而后,带有样品信息的离子碎片被加速进入质量分析器,不同的离子在质量分析器中被分离并按质荷比大小依次抵达检测器,经记录即得到按不同质荷比排列的离子质量谱,也就是质谱(massspectrum)。质谱:按离子的质荷比的大小依次排列形成的图谱质谱技术:M1M2(M1+1)+(M2+1)+(M1+1)+(M2+1)+离子源准分子离子(M+1)+多电荷离子(M+nH)n+质量分析器质谱分析系统的基本组成真空系统进样系统离子检测器数据采集系统离子源大气压质量分析器真空系统机械泵10-3-10-4torr(1atm=760torr)分子扩散泵10-6torr涡轮分子泵10-9torr离子泵10-11torr升华泵真空系统是任何MS的基础理想的真空系统是-高性能快速干净安全可靠离子检测器离子源数据采集质量分析器进样系统离子检测器离子源数据采集质量分析器进样系统储罐进样储气室、加热器、真空连接系统和分子漏孔色谱进样(气/液质联用)(气/液)相色谱出口直接导入探头进样样品室、玻璃毛细管,探头注射器进样毛细管电泳进样1电子轰击电离(EI)GC/MS2化学电离(CI)GC/MS3大气压化学电离(APCI)LC/MS4快原子/离子轰击(FAB/SIMS)离子源5等离子体解吸(PD)6基质辅助激光解吸电离(MALDI)7电喷雾电离(ESI)LC/MS8场致电离--Fieldionization9火花放电--Sparksource10激光电离--Laserionization(LIMS)11共振电离—Resonanceionization(RIMS)12热电离--Thermalionization(TIMS)离子检测器离子源数据采集进样系统质量分析器TurboTurboVVtmtm离子源离子源(API3200,API4000,(API3200,API4000,和和API5000)API5000)辅助气加热头TISorAPCI离子探头液体进入口垂直精密调节旋钮水平精密调节旋钮两通或三通离子源排气口喷雾针出口APCI电晕针TurboVTM离子源电喷雾(ESI)离子源工作原理电喷雾离子化分为三个过程:(液态带电)1形成带电小液滴2溶剂蒸发和小液滴碎裂3最终形成气相离子离子源的选择---ESI优点适合范围广:分析离子型/极性化合物、难挥发或热不稳定性化合物多电荷离子的形成,可以分析高分子量化合物灵敏度高缺点在溶液中必须形成离子流动相中缓冲盐的种类和浓度对灵敏度均有显著影响,因此流动相的选择非常重要具有流速依赖性基质抑制现象较为明显APCI三步离子化的过程(气态带电)1.溶剂快速蒸发形成气态分子2.电晕针放电使离子源内溶剂带电3.带电的溶剂离子与组分气态分子发生电荷转移,生成分子离子大气压化学电离源大气压化学电离源(APCI)(APCI)又叫又叫::加热雾化加热雾化源源HeatedNebulizerHeatedNebulizer离子源的选择---APCI优点有一定挥发性的中等极性或低极性的小分子化合物对溶剂选择、流速和添加物的依赖性较小缺点有可能发生热裂解样品需要有一定的挥发性适合分析分子量小于2000Da的样品离子源3.6e4Intensity,cpsMometasoneMinoxidilTIS0.51.01.52.02.53.03.5Time,min0.04.0e4Intensity,cps0.51.01.52.02.53.03.50.0Time,minMometasoneMinoxidilAPCI离子检测器离子源数据采集质量分析器进样系统1扇形磁场和静电场质量分析器2傅里叶变换离子回旋共振3飞行时间分析器4四极杆分析器5离子阱分析器+++++^_ABBAToDetector去检测器AABB离子簇在离子通道的运动模式电压使离子簇以螺旋运动的方式前进RFonly-Arods&Brodsare180outofphase只加交流信号---A杆与B杆上加的电压强度相同,相位差180度离子肼的工作原理离子肼的工作原理B应用制药:合成过程中中间体、成品的结构鉴定,杂质分析天然药物与中药分析:结构鉴定,质谱规律,中药药效物质基础药物代谢药物动力学:药动学药物代谢物寻找代谢组学蛋白组学(生物大分子分析)烟草食品分析公安毒物检查体育兴奋剂检测中药中非法添加化学药新生儿筛查制药行业合成过程中中间体、成品的结构初步鉴定杂质分析液质联用分析美伐他汀的有关物质制备液相分离,核磁确证结构天然产物与中药分析蟾酥药材HPLC/DAD/APCI-MS/MS定性定量分析方法从蟾酥药材中共鉴定了35个蟾毒内酯类成分,其中4个成分为首次发现。通过进一步实验,分别对17个蟾毒内酯类化合物进行多极质谱(MSn,n=2-4)裂解方式研究,根据化学结构和裂解规律将蟾毒内酯类化合物分为5类。蟾酥药材中8个主要蟾毒内酯类成分进行了定量分析。不仅可以快速、灵敏地分析蟾毒内酯类成分,还能够对蟾酥药材及相关制剂进行有效的质量控制。ZorbaxSB-C18色谱柱&保护柱流动相:(A)乙腈-(B)0.3%醋酸水溶液0-20min:A25%-30%,B75%-70%20-37min:A30%-50%,B70%-50%37-45min:A80%,B20%流速:1.0ml·min-1检测波长:275nm全波长扫描范围:190-400nm柱温:40℃液相色谱条件液相色谱条件质谱条件质谱条件ESI源负离子检测扫描范围:80-1000m/z鞘气流:50arb辅助气流:15arb源电压:5.00kV毛细管温度:350℃毛细管电压:-12.00V管透镜补偿电压:-10.00VHPLC-MS技术定性分析生物样品、降香药材中黄酮类成分HPLC-MS技术定性分析生物样品、降香药材中黄酮类成分4–methoxydalbergione260─40.9722prunetin26028338.4021pinocembrin232,29025537.4220medicarpin228,28626935.6919sativanone230,276,31029934.17183'-O-methylviolanone232,274,32032932.8917dalbergin232,35226731.7316formononetin250,30226731.1315isoliquiritigenin240,37225529.88142'-hydroxyformononetin248,29028323.6413vestitone278,31228520.8312butein26227119.1311violanone274,31031518.2710stevenin29031315.8992',7-dihydroxy-4',5'-dimethoxyisoflavone286,35028315.898melanettin29428313.807liquiritigenin230,276,31025512.546koparin240,29029911.585(3R)-4'-methoxy-2',3,7-trihydroxyisoflavanone28030110.4443'-hydroxymelanettin3402998.633butin232,2782717.9023'-hydroxydaidzein220,2922697.061Identityλmax(nm)[M-H]-(m/z)tR(min)No.采用HPLC-MS对黄酮类化合物对照品以及降香总黄酮的体外、体内分析结果RT:0.00-42.000510152025303540Time(min)-505101520253035404550556065707580859095100RelativeAbundance10.1838.2634.0523.6430.9611.5715.7937.4218.048.4929.8419.147.0935.7312.4020.8339.0825.604.261.44NL:1.27E7TICF:-cESISIMms[242.00-244.00,254.00-256.00,266.25-267.75,268.25-269.75,270.00-272.00,282.25-283.75,284.25-285.75,298.25-299.75,300.25-301.75,314.00-316.00]MS200411220212356789101112131415161718192021422RT:0.00-42.00024681012141618202224262830323436384042Time(min)020000400006000080000100000120000140000160000180000200000220000240000260000280000300000uAU32.8940.9731.7310.447.0634.177.9011.5815.8938.4012.5437.4231.1318.278.6320.8223.6435.6913.8019.1329.8840.582.642.9729.2725.734.270.33NL:3.17E5ChannelAUV200411220212345678910111213141516171819202122authenticcompounds(HPLC-UV)authenticcompounds(TIC-MS)对照品的HPLC-MS色谱图RT:0.00-42.000510152025303540Time(min)05101520253035404550556065707580859095100RelativeAbundance31.1233.9423.4818.1110.2020.6612.4629.7113.5915.858.5027.737.6524.9036.2037.337.0939.594.262.28NL:3.15E6TICF:-cESISIMms[242.00-244.00,254.00-256.00,266.25-267.75,268.25-269.75,270.00-272.00,282.25-283.75,284.25-285.75,298.25-299.75,300.25-301.75,314.00-316.00]MS200411220312345678910111213141517161819202122RT:0.00-42.00024681012141618202224262830323436384042Time(min)05000100001500020000250003000035000400004500050000uAU34.1812.537.8931.1320.8312.0632.8710.4318.275.9140.8213.8329.9035.7137.1723.678.6115.9339.2629.3919.157.0316.4427.933.5624.292.932.63NL:5.49E4ChannelAUV200411220312345678910111213141516171819202122thetotalflavonoidsofD.odorifera(HPLC-UV)thetotalflavonoidsofD.odorifera(TIC-MS)降香总黄酮的HPLC-MS色谱图RT:0.00-42.00024681012141618202224262830323436384042Time(min)05101520253035404550556065707580859095100RelativeAbundance41.2837.3236.7640.1539.5933.9314.709.3331.394.2426.0114.1421.4924.8829.1217.5310.4618.668.207.071.70NL:4.89E6TICF:-cESIFullms[50.00-800.00]MS2004112208RT:0.00-42.000510152025303540Time(min)05101520253035404550556065707580859095100RelativeAbundance10.4734.2131.1023.7515.8318.3812.4429.9720.928.505.6725.1636.7427.9938.444.262.28NL:7.81E6TICF:-cESISIMms[242.00-244.00,254.00-256.00,266.25-267.75,268.25-269.75,270.00-272.00,282.25-283.75,284.25-285.75,298.25-299.75,300.25-301.75,314.00-316.00]MS2004112207123456789101112131415161718RT:0.00-42.000510152025303540Time(min)05101520253035404550556065707580859095100RelativeAbundance10.2013.5523.4131.0312.4315.8033.8520.607.6618.068.2229.625.6827.6436.1137.2441.204.26NL:2.07E7TICF:-cESISIMms[242.00-244.00,254.00-256.00,266.25-267.75,268.25-269.75,270.00-272.00,282.25-283.75,284.25-285.75,298.25-299.75,300.25-301.75,314.00-316.00]MS2004112209123456789101112131415161718serumsamplewithenzymehydrolysisserumsamplewithouthydrolysisblankserum大鼠口服降香总黄酮后血清样品的TIC-MS色谱图1818血清TIC-MSRT:0.00-42.00024681012141618202224262830323436384042Time(min)05101520253035404550556065707580859095100RelativeAbundance41.0031.3823.7526.585.3729.4010.4633.0814.1418.9439.5822.6218.3834.2135.347.359.3315.8337.8911.590.292.83NL:2.29E6TICF:-cESIFullms[50.00-800.00]MS2004112206RT:0.00-42.000510152025303540Time(min)05101520253035404550556065707580859095100RelativeAbundance23.7610.2031.107.6624.3220.9413.8715.856.8132.8034.2118.3937.324.2629.9725.4538.74NL:4.50E6TICF:-cESISIMms[242.00-244.00,254.00-256.00,266.25-267.75,268.25-269.75,270.00-272.00,282.25-283.75,284.25-285.75,298.25-299.75,300.25-301.75,314.00-316.00]MS2004112204123456789101112131415171618RT:0.00-42.000510152025303540Time(min)05101520253035404550556065707580859095100RelativeAbundance23.7110.4613.847.6515.8112.4331.056.2420.905.6732.7418.3534.1625.684.2627.9437.2738.68NL:8.36E6TICF:-cESISIMms[242.00-244.00,254.00-256.00,266.25-267.75,268.25-269.75,270.00-272.00,282.25-283.75,284.25-285.75,298.25-299.75,300.25-301.75,314.00-316.00]MS2004112205123456789101112131415171618大鼠口服降香总黄酮后尿样的TIC-MS色谱图blankurineurinesamplewithouthydrolysisurinesamplewithenzymehydrolysis1818尿样TIC-MSRT:0.00-42.00024681012141618202224262830323436384042Time(min)05101520253035404550556065707580859095100RelativeAbundance41.2839.5838.7336.7534.7730.5334.2126.0122.6227.4213.5718.6619.7918.0913.0110.744.815.668.203.111.98NL:9.75E6TICF:-cESIFullms[50.00-800.00]MS2004112225RT:0.00-42.000510152025303540Time(min)05101520253035404550556065707580859095100RelativeAbundance31.6410.4824.5834.4618.9425.1412.7321.4816.4114.1430.5136.1436.9940.3828.534.267.93NL:9.82E6TICF:-cESISIMms[242.00-244.00,254.00-256.00,266.25-267.75,268.25-269.75,270.00-272.00,282.25-283.75,284.25-285.75,298.25-299.75,300.25-301.75,314.00-316.00]MS2004112213234567891011121314151718RT:0.00-42.000510152025303540Time(min)05101520253035404550556065707580859095100RelativeAbundance31.6410.4834.4624.3118.9514.1412.7325.1416.4121.4830.5128.5336.147.9437.847.095.67NL:8.60E6TICF:-cESISIMms[242.00-244.00,254.00-256.00,266.25-267.75,268.25-269.75,270.00-272.00,282.25-283.75,284.25-285.75,298.25-299.75,300.25-301.75,314.00-316.00]MS2004112214234567891011121314151718大鼠口服降香总黄酮后肝脏样品的TIC-MS色谱图blankliverliversamplewithouthydrolysisliversamplewithenzymehydrolysis1616肝脏TIC-MSRT:0.00-42.00024681012141618202224262830323436384042Time(min)05101520253035404550556065707580859095100RelativeAbundance41.0034.7831.1030.5334.2137.6010.7529.6926.2916.1221.7724.889.9015.2720.646.7918.105.09NL:8.91E6TICF:-cESIFullms[50.00-800.00]MS2004112226RT:0.00-42.000510152025303540Time(min)05101520253035404550556065707580859095100RelativeAbundance31.6910.4824.3434.5118.6812.7421.5116.4214.1630.2725.184.267.9440.4537.917.0928.58NL:2.62E6TICF:-cESISIMms[242.00-244.00,254.00-256.00,266.25-267.75,268.25-269.75,270.00-272.00,282.25-283.75,284.25-285.75,298.25-299.75,300.25-301.75,314.00-316.00]MS200411221523456789101112131415171816RT:0.00-42.000510152025303540Time(min)05101520253035404550556065707580859095100RelativeAbundance31.6710.4824.6114.1534.4918.9612.7416.4121.5030.547.947.095.6841.0036.194.2639.3028.56NL:5.28E6TICF:-cESISIMms[242.00-244.00,254.00-256.00,266.25-267.75,268.25-269.75,270.00-272.00,282.25-283.75,284.25-285.75,298.25-299.75,300.25-301.75,314.00-316.00]MS2004112216234567891011121314151718161blankkidneykidneysamplewithouthydrolysiskidneysamplewithenzymehydrolysis大鼠口服降香总黄酮后肾脏样品的TIC-MS色谱图1718肾脏TIC-MSRT:0.00-42.00024681012141618202224262830323436384042Time(min)05101520253035404550556065707580859095100RelativeAbundance41.3040.7330.5431.1139.0334.7936.4934.2232.2416.1228.8427.7125.4524.3218.3814.9921.4911.038.496.514.81NL:1.14E7TICF:-cESIFullms[50.00-800.00]MS2004112229RT:0.00-42.000510152025303540Time(min)05101520253035404550556065707580859095100RelativeAbundance31.6910.4834.5224.6212.7421.5125.1938.7736.7814.1618.9616.704.266.807.6529.14NL:1.76E6TICF:-cESISIMms[242.00-244.00,254.00-256.00,266.25-267.75,268.25-269.75,270.00-272.00,282.25-283.75,284.25-285.75,298.25-299.75,300.25-301.75,314.00-316.00]MS2004112220461213151718RT:0.00-42.000510152025303540Time(min)05101520253035404550556065707580859095100RelativeAbundance31.6910.4934.5224.3414.1612.7421.5116.4218.9725.1941.027.9437.066.8128.595.685.113.13NL:3.12E6TICF:-cESISIMms[242.00-244.00,254.00-256.00,266.25-267.75,268.25-269.75,270.00-272.00,282.25-283.75,284.25-285.75,298.25-299.75,300.25-301.75,314.00-316.00]MS2004112222461213151718blanklunglungsamplewithouthydrolysislungsamplewithenzymehydrolysis大鼠口服降香总黄酮后肺脏样品的TIC-MS色谱图77肺脏TIC-MSRT:0.00-42.00024681012141618202224262830323436384042Time(min)05101520253035404550556065707580859095100RelativeAbundance41.2830.8234.7834.2138.4637.6133.3628.8427.7110.7411.8725.7318.9416.685.6613.5723.1820.647.077.92NL:1.49E7TICF:-cESIFullms[50.00-800.00]MS2004112227RT:0.00-42.000510152025303540Time(min)05101520253035404550556065707580859095100RelativeAbundance31.7010.4834.5224.3421.5118.9716.4212.7525.7641.0337.076.814.2627.469.3529.44NL:2.35E6TICF:-cESISIMms[242.00-244.00,254.00-256.00,266.25-267.75,268.25-269.75,270.00-272.00,282.25-283.75,284.25-285.75,298.25-299.75,300.25-301.75,314.00-316.00]MS20041122194612131517189107RT:0.00-42.000510152025303540Time(min)05101520253035404550556065707580859095100RelativeAbundance31.7010.4934.5324.3521.5214.1641.3120.1016.4325.766.8138.2118.414.2627.46NL:1.74E6TICF:-cESISIMms[242.00-244.00,254.00-256.00,266.25-267.75,268.25-269.75,270.00-272.00,282.25-283.75,284.25-285.75,298.25-299.75,300.25-301.75,314.00-316.00]MS2004112221461213151718910大鼠口服降香总黄酮后心脏样品的TIC-MS色谱图blankheartheartsamplewithouthydrolysisheartsamplewithenzymehydrolysis1010心脏TIC-MSRT:0.00-42.00024681012141618202224262830323436384042Time(min)05101520253035404550556065707580859095100RelativeAbundance31.1038.4534.7836.4731.6629.4028.8424.0316.4021.7712.1618.6610.747.9214.424.525.66NL:1.07E7TICF:-cESIFullms[50.00-800.00]MS2004112228RT:0.00-42.000510152025303540Time(min)05101520253035404550556065707580859095100RelativeAbundance31.6910.4834.5241.0324.3421.5116.7136.5120.1012.7538.7713.8818.684.2625.757.6628.58NL:1.55E6TICF:-cESISIMms[242.00-244.00,254.00-256.00,266.25-267.75,268.25-269.75,270.00-272.00,282.25-283.75,284.25-285.75,298.25-299.75,300.25-301.75,314.00-316.00]MS2004112217461213151718RT:0.00-42.000510152025303540Time(min)05101520253035404550556065707580859095100RelativeAbundance31.6910.4834.5224.3414.1621.5112.7416.4218.9725.1941.0339.346.804.268.5030.00NL:1.97E6TICF:-cESISIMms[242.00-244.00,254.00-256.00,266.25-267.75,268.25-269.75,270.00-272.00,282.25-283.75,284.25-285.75,298.25-299.75,300.25-301.75,314.00-316.00]MS20041122184612131517187891016大鼠口服降香总黄酮后脾脏样品的TIC-MS色谱图blankspleenspleensamplewithouthydrolysisspleensamplewithenzymehydrolysis712脾脏TIC-MS中药制剂中掺入西药成分分析液质联用分析中药降糖制剂中掺入的西药成分药物代谢与药物动力学Max.75.0cps.1234567Time,min01020304050607075Intensity,cps5.855.92Max.90.0cps.1234567Time,min0102030405060708090Intensity,cpsMax.866.9cps.1234567Time,min0100200300400500600700800867Intensity,cps6.555.83Max.5.8e4cps.1234567Time,min0.05000.01.0e41.5e42.0e42.5e43.0e43.5e44.0e44.5e45.0e45.5e45.8e4Intensity,cps4.53Intensity,cpsIntensity,cpsIntensity,cpsIntensity,cpsMax.6.1e4cps.1234567Time,min0.05000.01.0e41.5e42.0e42.5e43.0e43.5e44.0e44.5e45.0e45.5e46.0e4Intensity,cps6.535.83Max.4.8e4cps.1234567Time,min0.05000.01.0e41.5e42.0e42.5e43.0e43.5e44.0e44.5e44.8e4Intensity,cps4.53(A)(A)ⅡⅠⅠⅡⅢⅢ(B)(B)(C)(C)空白血浆样空白血浆样品色谱图品色谱图空白血浆添加内酯苷和芍药苷的色谱图大鼠灌服白芍总苷溶液后血浆样品色谱图内酯苷内酯苷栀子苷栀子苷芍药苷芍药苷5.836.554.53芍药苷和芍药内酯苷同时测定多离子反应监测色谱图芍药苷和芍药内酯苷同时测定多离子反应监测色谱图白芍总苷药动学研究白芍总苷药动学研究给予大鼠白芍总苷水溶液,剂量给予大鼠白芍总苷水溶液,剂量162mg/kg162mg/kg,,相当相当于芍药苷于芍药苷53.36mg/kg53.36mg/kg和和15.21mg/kg15.21mg/kg。。单体给药和给予白芍总苷后芍药苷药动学参数比较,单体给药和给予白芍总苷后芍药苷药动学参数比较,CCmaxmax、、TmaxTmax无显无显著性差异,著性差异,AUCAUC0-0-tt、、tt½½有有显著性差异。说明芍药苷动力学过程受白芍显著性差异。说明芍药苷动力学过程受白芍总苷中其他成分的影响。总苷中其他成分的影响。020040060080010001200050100150200250300350400Time(min)Concentration(ng/ml)单体芍药苷白芍总苷比较低剂量芍药内酯苷单体和白芍总苷的药动学参数,结果表明比较低剂量芍药内酯苷单体和白芍总苷的药动学参数,结果表明两种给药形式下芍药内酯苷的两种给药形式下芍药内酯苷的CCmaxmax、、TTmaxmax、、AUCAUC0-t0-t与与tt1/21/2之间无显著之间无显著性差异,即芍药内酯苷药物动力学过程不受白芍总苷中其他成分性差异,即芍药内酯苷药物动力学过程不受白芍总苷中其他成分的影响。的影响。-50050100150200250300350400450050100150200250300350400Time(min)Concentration(ng/ml)单体芍药内酯苷白芍总苷中药药效物质基础与配方原则研究单煎液和共煎液汤剂复方配伍原则君(King):提供主要治疗作用臣(Minister)佐(Assistant)起加强,调和,辅助君药功能的作用使(Servant)化学反应传统中药附子(TherootsofAconitumCarmichaelidebx,RAC)在中国被广泛用于抗风湿、止痛等RAC,君臣佐使XXXBletillapinelliafrilillary白芨半夏贝母+liquoricegingerwhitepenoy甘草干姜白芍为增效减毒,附子经常与甘草(liquorice),干姜(ginger),白芍,(whitepeony)和人参等(ginseng)共同使用(这里称第一类中药,groupI),尤其是甘草,中医千百年的医疗实践表明它具有广泛的解毒作用与一类中药相反,半夏(pinelliatuber),贝母(frilillarybulb)或白芨(bletillatuber)等禁止与附子共用,这里称第二类中药(groupIIofherbs)含附子组方的配伍原则含附子组方的配伍原则质谱分析1.通过ESI-MS,鉴定了生附子中的生物碱:双酯型生物碱及脂碱的结构2.附子煎煮前后所含生物碱的对比以及煎煮过程中所发生的反应3.附子与其他草药共煎生物碱含量的变化4.pH值对于反应的影响5005506006507007508008509009501000m/z0102030405060708090100RelativeAbundance5005506006507007508008509009501000m/z0102030405060708090100RelativeAbundance590616866852648868574632812836BMBH604BAHAMABW662AF590616866852648868574632812836BMBH604BAHAMABW662AF590616866852648868574632812836BMBH604BAHAMABW662AF590616866852648868574632812836BMBH604BAHAMABW662AF590616866852648868574632812836BMBH604BAHAMABW662AF590616866852648868574632812836BMBH604BAHAMABW662AF5005506006507007508008509009501000m/z0102030405060708090100RelativeAbundance5005506006507007508008509009501000m/z0102030405060708090100RelativeAbundance590604648574866662836812616868852BMBAHABWAFHAPHALMALACLACO附子+水附子+甘草DDAMDADDAMDA5005506006507007508008509009501000m/z0102030405060708090100RelativeAbundance5005506006507007508008509009501000m/z0102030405060708090100RelativeAbundance648632590662572604616646AFBWACHABABMBM-H2O附子+半夏DDAMDA公安、司法鉴定公安、司法鉴定LC-MS/MS技术在法庭科学中的应用毒品/滥用药物:可卡因、海洛因、吗啡、摇头丸、迷幻药等等2001年1-6月缴获海洛因6201千克、鸦片1927千克、冰毒2970千克、摇头丸64万粒、度冷丁1400支、咖啡因80千克、罂粟壳40吨、易制毒化学品72吨毒物:鼠药、农药、工业毒物、药物毒物、蛇/蝎/蜂毒、河豚毒素及其它海洋生物毒素、植物毒素等等爆炸物:硝化甘油、OCTOGEN、HMX、EGDN、HEXOGEN、RDX、NG、TETRYL、DNT和PETN等等其它化合物:案发现场遗物如油漆、血迹、高聚物等质谱在生物大分子研究领域中的应用1蛋白质和多肽的分析2寡核苷酸和核酸的分析3微生物鉴定4药物 设计 领导形象设计圆作业设计ao工艺污水处理厂设计附属工程施工组织设计清扫机器人结构设计 5多糖结构测定蛋白质和多肽的分析分子量测定肽谱测定肽及蛋白质序列测定巯基和二硫键定位蛋白质翻译后修饰分析抗原决定部位指认生物分子相互作用及非共价复合物分析液质联用蛋白质组学鉴定方法的建立其在正常人尿蛋白质组鉴定中的应用(中国协和医科大学博士论文)液质联用分析重组人白细胞介素2的肽图(药学学报2006,41(8):756–760)新生儿筛查新生儿筛查新生儿筛查是对一些目前还无法在产前做出诊断的先天性代谢性疾病及内分泌疾病在新生儿进行普查,以筛选出病人,提前做出诊断,提前进行治疗Why?这些先天性疾病疾病目前在出生以前用产前检查的方法还无法诊断,婴儿出生以前又没有有病的迹象一旦出现异常情况以后,身体和智力已经受到不可逆转的损害,失去治疗的机会为了对这些疾病做出早期诊断,从60年代起。欧美一些国家和日本等国开展了新生儿筛查工作,多年以来,这是一种行之有效的措施。通常的化验方法是采血和采尿现在新生儿筛查主要是针对:1.先天性甲状腺功能低下(服用甲状腺激素可以完全避免痴呆的发生)2.苯丙酮尿症(只要不服用含有苯丙氨酸的包括人奶在内的食品就可以完全避免痴呆的发生)3.半乳糖血症(只要不服用含有乳糖的包括人奶在内的食品就可以完全避免痴呆的发生)新生儿筛查的一般过程:2.100ul甲醇溶液( 标准 excel标准偏差excel标准偏差函数exl标准差函数国标检验抽样标准表免费下载红头文件格式标准下载 )1.取样3.上清液50℃吹干4.50ul正丁醇溶液衍生5.吹干,再溶解35ul总结分离分析(强大)定性、定量不仅仅是检测器,HPLC是其进样装置。用于单一物质、混合物有机物的结构鉴定、定量分析药学院:3200Qtrap,欢迎使用!谢谢!药学院药物分析教研室王巧0311-86265625AnyQuestions??
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