CAJ | 학술논문

构建微流蒸发光散射检测器(μELSD)与加压毛细管电色谱( pCEC)联用系统,测定中药提取物注射用血塞通(冻干)中三七皂苷R1、人参皂苷Rg1, Re, Rb1、Rd考察系统的实用性和稳定性。用C18毛细管色谱柱,通过对流动相体系、梯度洗脱条件、雾化载气流速、蒸发温度、施加电压等参数的优化,确定了注射用血塞通(冻干)5种成分含量测定的最佳测定参数。最佳测定参数如下,流动相A为15 mmol/L甲酸-三乙胺乙腈溶液(pH=7.0),流动相B为15 mmol/L甲酸-三乙胺溶液(pH=7.0)；梯度洗脱条件：0~10 min,19%A；10~30 min,22%A；30~35 min,36%A；35~45 min,40%A。雾化载气流速2 L/min；蒸发温度120℃；施加电压+8 kV。5种成分线性范围为8.6~146.9 ng (三七皂苷 R1)、6.9~189.7 ng (人参皂苷 Rg1)、6.8~171.4 ng(人参皂苷Re)、9.4~156.1 ng(人参皂苷Rb1)、7.5~180.5 ng(人参皂苷Rd),5种成分回收率都在95%~105%之间。实验表明,构建的pCEC-μELSD联用系统能用于药物中有效成分的含量测定。μELSD的构建为毛细管液相色谱、毛细管电色谱和毛细管电泳分离技术提供了一种全新的检测手段。
구건미류증발광산사검측기(μELSD)여가압모세관전색보( pCEC)련용계통,측정중약제취물주사용혈새통(동간)중삼칠조감R1、인삼조감Rg1, Re, Rb1、Rd고찰계통적실용성화은정성。용C18모세관색보주,통과대류동상체계、제도세탈조건、무화재기류속、증발온도、시가전압등삼수적우화,학정료주사용혈새통(동간)5충성분함량측정적최가측정삼수。최가측정삼수여하,류동상A위15 mmol/L갑산-삼을알을정용액(pH=7.0),류동상B위15 mmol/L갑산-삼을알용액(pH=7.0)；제도세탈조건：0~10 min,19%A；10~30 min,22%A；30~35 min,36%A；35~45 min,40%A。무화재기류속2 L/min；증발온도120℃；시가전압+8 kV。5충성분선성범위위8.6~146.9 ng (삼칠조감 R1)、6.9~189.7 ng (인삼조감 Rg1)、6.8~171.4 ng(인삼조감Re)、9.4~156.1 ng(인삼조감Rb1)、7.5~180.5 ng(인삼조감Rd),5충성분회수솔도재95%~105%지간。실험표명,구건적pCEC-μELSD련용계통능용우약물중유효성분적함량측정。μELSD적구건위모세관액상색보、모세관전색보화모세관전영분리기술제공료일충전신적검측수단。
A novel separation system of microflow evaporative light scattering detector (μELSD) coupled with pressurized capillary electrochromatography ( pCEC) was built and applied to the separation and detection of notoginsenoside R1 , ginsenoside Rg1 , ginsenoside Re, ginsenoside Rb1 , ginsenoside Rd in traditional Chinese medicine extract Xuesaitong (lyophilization). With C18 capillary column the best separation conditions were established by optimizing the mobile phase composition, gradient conditions, flow rate of atomizing gas, evaporating temperature and applied voltage. The mobile phase A was acetonitrile containing 15 mmol/L formic acid-triethylamine acetonitrile ( pH=7 . 0 ) , and the mobile phase B was 15 mmol/L formic acid-triethylamine acetonitrile (pH=7. 0). The optimized gradient elution conditions were as follows:0-10 min, 19%A;10-30 min, 22%A;30-35 min, 36%A;35-45 min, 40%A. The flow rate of atomizing gas( N2 ) was 2 L/min. The evaporating temperature was 120 ℃. The applied voltage was+8 kV. A good linearity was obtained:8. 6-146. 9 ng ( notoginsenoside R1 ), 6. 9-189. 7 ng ( ginsenoside Rg1 ), 6. 8-171. 4 ng (ginsenoside Re), 9. 4-156. 1 ng (ginsenoside Rb1), 7. 5-180. 5 ng (ginsenoside Rd). The recovery was between 95%-105%. The results show that the pCEC-μELSD system can be used for the determination of the content of active ingredients in medicines. The construction ofμELSD provides an innovative detection means for capillary liquid chromatography, pCEC and capillary electrophoresis.