蒸發(fā)光散射檢測器

1、樣品量響應(yīng)值SxBCA l 不同物質(zhì)的量值響應(yīng)曲線的斜率與物質(zhì)的不同物質(zhì)的量值響應(yīng)曲線的斜率與物質(zhì)的本身結(jié)構(gòu)有關(guān)。本身結(jié)構(gòu)有關(guān)。 NSNHH2NOOOOHCH3HHH頭孢拉定頭孢拉定NSNHH2NOOOOHCH3HHH頭孢氨芐頭孢氨芐NSNHH2NOOOOHHHHCl頭孢克洛頭孢克洛頭孢拉定頭孢克洛580563583651OHOOHOONH2OHNHHR2HR1OHCH3CH3OHOOOOHOOHCH3CH3NHNH2CHNH2NH213NHR1R2名稱R1R2雙鍵*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對曲線y = 1.461x + 5.0667R2 = 0.99954.855.25.45.65.86-0.200.20.40.60.8進(jìn)樣量（微克）的常用對數(shù)峰響應(yīng)值的常用對數(shù)依替米星校對曲線y = 1.4611x + 4.8528R2 = 0.99994.855.25.45.65.8600.20.40.60.8進(jìn)樣量（微克）的常用對數(shù)峰響應(yīng)值的常用對數(shù)誤差來源f(x-x)2(x-x)(y-y)(y-y)2b離差分析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50.2370.3300.4671.39040.007510.00188二組誤差和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進(jìn)樣量（ug）ELSD峰面積頭孢氨芐頭孢拉定頭孢克洛頭孢唑啉頭孢替唑頭孢拉定頭孢克洛580563583651 x0（最低檢出限）0y-mykxm曲線部分名稱直線方程相關(guān)系數(shù)(R2)含量實驗線性起點ug實驗線性終點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麥迪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、稱直線方程相關(guān)系數(shù)R2含量實驗線性起點ug實驗線性終點ug頭孢氨芐y = 579824 x - 10862111.000093.2%4.3921.97頭孢克洛y = 548632 x - 9105970.999694.0%4.2921.44頭孢拉定y = 532957 x - 1077897 0.999591.8%4.5322.65頭孢唑啉y = 529897 x - 12595660.999499.3%4.2721.35頭孢替唑y = 493704 x - 10536470.999593.0%4.2221.10諾氟沙星y = 670899 x - 11469060.999598.9%5.86

7、29.30左氟沙星y = 648130 x - 14012870.999797.2%5.8028.98依諾沙星y = 575780 x - 1328730 0.999391.1%8.2841.41洛美沙星y = 552908 x - 15382100.999790.0%5.3426.71環(huán)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進(jìn)樣量峰面積威替米星諾氟沙星依諾沙星環(huán)丙沙星左氟沙星麥迪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進(jìn)樣量的常用對數(shù)峰面積常用對數(shù)威替米星諾氟沙星依諾沙星環(huán)丙沙星左氟沙星麥迪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進(jìn)樣量峰面積威

11、替米星諾氟沙星依諾沙星環(huán)丙沙星左氟沙星麥迪A1洛美沙星名稱線性起點g線性終點g直接線性R2雙對數(shù)線性R2多項式線性R2威替米星2.4618.470.99970.99530.9998諾氟沙星0.6212.370.99500.99500.9996依諾沙星0.6713.450.99210.99870.9997環(huán)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麥迪A11.0613.300.99310.99790.9999圖3-1 漂移管溫度優(yōu)化 圖3-2 載氣流速優(yōu)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、機 相 含 量 （ ）UV峰面積麥 迪 A 1 U V 峰 面 積交 沙 U V 峰 面 積圖3-3A 不同有機相含量下麥迪A1及交沙霉素UV峰面積變化圖 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 機 相 含 量 （ ）ELSD峰面積麥 迪 A 1 E L S D 峰 面 積交 沙 E L S D 峰 面

14、積圖3-3B 不同有機相含量下麥迪A1及交沙霉素ELSD峰面積變化圖 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%有機相含量（）低進(jìn)樣量ELSD峰面積010000002000000300000040000005000000600

15、000070000008000000900000010000000高進(jìn)樣量ELSD峰面積麥迪A1低交沙霉素麥迪A1高圖3-4 不同進(jìn)樣量的麥迪A1以及交沙霉素ELSD峰面積 與流動相中有機相含量線性方程表表3-2 3-2 流動組成微小變化對流動組成微小變化對ELSDELSD響應(yīng)影響的模擬計算結(jié)果響應(yīng)影響的模擬計算結(jié)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圖3-7 20mmol/L與4mmol/L NH4Ac溶液在ELSD離柱分析中的色譜疊加圖 xym0mkxy)(0最低檢測限x曲線部分曲線部分RxRxAACC)(含量 mAmACCRxRx)(含量 mkxykxy 0mRxAA xARARxAA NiiiAiAiC17 .1/17 .1/1)()(品名品名位置位置項目項目流動相流動相參考參考ELSDELSD條條件件相關(guān)相關(guān)硫 酸 小硫 酸 小諾霉素諾霉素ChPIC

18、hPI-718-718鑒別、組分檢鑒別、組分檢查查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鑒別、卡拉鑒別、卡拉B B檢查、含測檢查、含測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 慶硫 酸 慶大霉素大霉素ChPIChPI-730-730C

19、C組分檢查組分檢查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鑒別、含測鑒別、含測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項目項目流動相流動相黃芪黃芪ChPII-ChPII-212212含測（黃芪甲苷）含測（黃芪甲苷）乙腈乙腈- -水水(32:68)(32:68)炙黃芪炙黃芪ChPII-ChPII-213213 同黃芪同黃芪 同黃芪同黃芪銀杏葉銀杏葉ChPII-ChPII-2202