蒸发光散射检测器

1、样品量响应值SxBCA l 不同物质的量值响应曲线的斜率与物质的不同物质的量值响应曲线的斜率与物质的本身结构有关。本身结构有关。 NSNHH2NOOOOHCH3HHH头孢拉定头孢拉定NSNHH2NOOOOHCH3HHH头孢氨苄头孢氨苄NSNHH2NOOOOHHHHCl头孢克洛头孢克洛头孢拉定头孢克洛580563583651OHOOHOONH2OHNHHR2HR1OHCH3CH3OHOOOOHOOHCH3CH3NHNH2CHNH2NH213NHR1R2名称R1R2双键*西索米星HH奈替米星-C2H5H+威替米星-C2H5-CH3+依替米星-C2H5HHONH2NHOOONH2OCH2OHOHNH

2、2HOOOHHOHOCH2 NH2HOH阿米卡星阿米卡星校对曲线y = 1.461x + 5.0667R2 = 0.99954.855.25.45.65.86-0.200.20.40.60.8进样量（微克）的常用对数峰响应值的常用对数依替米星校对曲线y = 1.4611x + 4.8528R2 = 0.99994.855.25.45.65.8600.20.40.60.8进样量（微克）的常用对数峰响应值的常用对数误差来源f(x-x)2(x-x)(y-y)(y-y)2b离差分析f平方和均方F值P奈替米星50.2340.3550.5401.51740.001430.0003585.250.05威替米

3、星50.2370.3300.4671.39040.007510.00188二组误差和80.008940.00112公共坡度100.4710.6851.0071.45490.01080.0012平行性10.001860.001861.660.05NNOCOOHHNNFC2H5NOCOOHNNFOCH3H3CNOCOOHHNNFNOCOOHHNNFCH2CH3FCH3NOCOOHHNNFOCH3CH3y = 579824.5 x - 1086211R2 = 1.0000y = 548632x - 910597R2 = 0.9996y = 532957 x - 1077897R2 = 0.9995y

4、 = 493704 x - 1053647R2 = 0.9995y = 529897 x - 1259566R2 = 0.99940.E+002.E+064.E+066.E+068.E+061.E+071.E+071.E+07051015202530进样量（ug）ELSD峰面积头孢氨苄头孢拉定头孢克洛头孢唑啉头孢替唑头孢拉定头孢克洛580563583651 x0（最低检出限）0y-mykxm曲线部分名称直线方程相关系数(R2)含量实验线性起点ug实验线性终点g阿米卡星y = 581559 x - 6011550.9997/1.7521.82威替米星y = 372803 x - 4658560.

5、9999/4.9230.78SCO-4y = 297467 x - 3941651.0000/4.7829.85麦迪A1y = 466980 x - 12234830.999895.9%2.5551.00吉他A5y = 186483 x - 1143668 0.999940.2%7.51/吉他A4y = 71031x - 9584340.999715.5%5.79/吉他A1y = 26294x - 3331480.99917.5%2.80/吉他A7y = 24357x - 3503980.99925.4%2.02/吉他A13y = 21561x - 3948340.99966.6%2.47/名

6、称直线方程相关系数R2含量实验线性起点ug实验线性终点ug头孢氨苄y = 579824 x - 10862111.000093.2%4.3921.97头孢克洛y = 548632 x - 9105970.999694.0%4.2921.44头孢拉定y = 532957 x - 1077897 0.999591.8%4.5322.65头孢唑啉y = 529897 x - 12595660.999499.3%4.2721.35头孢替唑y = 493704 x - 10536470.999593.0%4.2221.10诺氟沙星y = 670899 x - 11469060.999598.9%5.86

7、29.30左氟沙星y = 648130 x - 14012870.999797.2%5.8028.98依诺沙星y = 575780 x - 1328730 0.999391.1%8.2841.41洛美沙星y = 552908 x - 15382100.999790.0%5.3426.71环丙沙星y = 536791 x - 12274030.999884.2%6.8234.08y = 615365 x - 565619R2 = 0.9950y = 590869x - 699605R2 = 0.9923y = 486349x - 519954R2 = 0.9921y = 493505x - 61

8、9236R2 = 0.996y = 370004x - 433940R2 = 0.9997y = 382652x - 383585R2 = 0.9931y = 469321x - 746364R2 = 0.9946-20000000200000040000006000000800000010000000120000000.05.010.015.020.025.0进样量峰面积威替米星诺氟沙星依诺沙星环丙沙星左氟沙星麦迪A1洛美沙星y = 1.4797 x + 5.2948R2 = 0.9950y = 1.4988x + 5.2089R2 = 0.9982y = 1.4408x + 5.1938R

9、2 = 0.9987y = 1.3917x + 5.2121R2 = 0.9964y = 1.2704x + 5.227R2 = 0.9953y = 1.2407x + 5.2675R2 = 0.9979y = 1.3904x + 5.1507R2 = 0.99914.55.05.56.06.57.07.5-0.4-0.20.00.20.40.60.81.01.21.41.6进样量的常用对数峰面积常用对数威替米星诺氟沙星依诺沙星环丙沙星左氟沙星麦迪A1洛美沙星y = 13279x2 + 438198x - 254393R2 = 0.9996y = 13576x2 + 383515x - 282

10、615R2 = 0.9992y = 12370 x2 + 306837x - 176948R2 = 0.9997y = 6330.3x2 + 363604x - 268248R2 = 0.9998y = 5796x2 + 332484x - 320997R2 = 0.9993y = 10874x2 + 219306x - 51169R2 = 0.9999y = -491.99x2 + 380420 x - 472013R2 = 0.9998-2.E+060.E+002.E+064.E+066.E+068.E+061.E+071.E+070.05.010.015.020.025.0进样量峰面积威

11、替米星诺氟沙星依诺沙星环丙沙星左氟沙星麦迪A1洛美沙星名称线性起点g线性终点g直接线性R2双对数线性R2多项式线性R2威替米星2.4618.470.99970.99530.9998诺氟沙星0.6212.370.99500.99500.9996依诺沙星0.6713.450.99210.99870.9997环丙沙星0.9519.020.99600.99640.9998左氟沙星0.7114.160.99230.99820.9992洛美沙星1.0921.880.99460.99910.9993麦迪A11.0613.300.99310.99790.9999图3-1 漂移管温度优化 图3-2 载气流速优化

12、00.40.81.21.6120115110105Temperature of the drift tube / Background noise (mV)00.20.40.60.83.062.82.682.55Flow of carrier gas/L min-10 . E + 0 01 . E + 0 62 . E + 0 63 . E + 0 64 . E + 0 65 . E + 0 66 . E + 0 67 . E + 0 68 . E + 0 69 . E + 0 61 . E + 0 75 6 . 2 5 %5 2 . 5 0 %5 0 . 0 0 %4 7 . 5 0 %有

13、机 相 含 量 （ ）UV峰面积麦 迪 A 1 U V 峰 面 积交 沙 U V 峰 面 积图3-3A 不同有机相含量下麦迪A1及交沙霉素UV峰面积变化图 0 . E + 0 01 . E + 0 52 . E + 0 53 . E + 0 54 . E + 0 55 . E + 0 56 . E + 0 57 . E + 0 58 . E + 0 59 . E + 0 51 . E + 0 65 6 . 2 5 %5 2 . 5 0 %5 0 . 0 0 %4 7 . 5 0 %有 机 相 含 量 （ ）ELSD峰面积麦 迪 A 1 E L S D 峰 面 积交 沙 E L S D 峰 面

14、积图3-3B 不同有机相含量下麦迪A1及交沙霉素ELSD峰面积变化图 y = 39167330 x - 12692628R2 = 0.9901y = 6720157 x - 2863327R2 = 0.9972y = 5040274 x - 1997100R2 = 0.99510100000200000300000400000500000600000700000800000900000100000046.00%48.00%50.00%52.00%54.00%56.00%58.00%有机相含量（）低进样量ELSD峰面积010000002000000300000040000005000000600

15、000070000008000000900000010000000高进样量ELSD峰面积麦迪A1低交沙霉素麦迪A1高图3-4 不同进样量的麦迪A1以及交沙霉素ELSD峰面积 与流动相中有机相含量线性方程表表3-2 3-2 流动组成微小变化对流动组成微小变化对ELSDELSD响应影响的模拟计算结果响应影响的模拟计算结果23.21min20406080100120140160Temperature (C)-101030507090110Weight (%)0510152025Time (min)Sample: (NH)4ACSize: 38.0380 mgMethod: mashihongTGAF

16、ile: C:TADataTGAmshNH4Ac.zdsOperator: wzjRun Date: 5-Apr-04 18:33Instrument: 2950 TGA HR V5.4AUniversal V3.4C TA Instruments-12.22%/min20406080100120140Temperature (C)-101030507090110Weight (%)0246810121416Time (min)Sample: (NH)4ACSize: 30.1310 mgMethod: mashihongTGAFile: C:TADataTGAmshNH4Ad.zdsOper

17、ator: wzjRun Date: 5-Apr-04 19:27Instrument: 2950 TGA HR V5.4AUniversal V3.4C TA Instruments图3-7 20mmol/L与4mmol/L NH4Ac溶液在ELSD离柱分析中的色谱叠加图 xym0mkxy)(0最低检测限x曲线部分曲线部分RxRxAACC)(含量 mAmACCRxRx)(含量 mkxykxy 0mRxAA xARARxAA NiiiAiAiC17 .1/17 .1/1)()(品名品名位置位置项目项目流动相流动相参考参考ELSDELSD条条件件相关相关硫 酸 小硫 酸 小诺霉素诺霉素ChPIC

18、hPI-718-718鉴别、组分检鉴别、组分检查查0.2M TFA-0.2M TFA-M(94:6)M(94:6)T : 1 1 0T : 1 1 0 C C F:2.8L/minF:2.8L/min口服液、片、口服液、片、注射液注射液硫 酸 卡硫 酸 卡拉霉素拉霉素ChPIChPI-724-724鉴别、卡拉鉴别、卡拉B B检查、含测检查、含测0.2M TFA-0.2M TFA-M(95:5)M(95:5)T : 1 1 0T : 1 1 0 C C F:3L/minF:3L/min注射液、滴眼注射液、滴眼液、注射用液、注射用硫 酸 庆硫 酸 庆大霉素大霉素ChPIChPI-730-730C

19、C组分检查组分检查0.2M TFA-0.2M TFA-M(92:8)M(92:8)T : 1 1 0T : 1 1 0 C C F:2.8L/minF:2.8L/min注射液注射液硫 酸 依硫 酸 依替米星替米星ChPIChPI-740-740鉴别、含测鉴别、含测0.2M TFA-0.2M TFA-M(84:16)M(84:16)T : 1 0 0T : 1 0 0 C C F:1.6L/minF:1.6L/min注射液、注射注射液、注射用用品名品名位置位置项目项目流动相流动相黄芪黄芪ChPII-ChPII-212212含测（黄芪甲苷）含测（黄芪甲苷）乙腈乙腈- -水水(32:68)(32:68)炙黄芪炙黄芪ChPII-ChPII-213213 同黄芪同黄芪 同黄芪同黄芪银杏叶银杏叶ChPII-ChPII-2202