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建立了超高效液相色谱-串联质谱法同时测定复方罗布麻片Ⅰ中的氢氯噻嗪(1)、防己诺林碱(2)、粉防己碱(3)、芦丁(4)、金丝桃苷(5)、氯氮?(6)和异丙嗪(7)。采用Acquity UPLC HSS C18色谱柱,以水∶甲醇(均含0.01%甲酸)为流动相,梯度洗脱。采用多反应监测,结合正负离子分段扫描。2、3、6、7采用正离子模式,1、4、5采用负离子模式。1~7分别在0.770~48.650、0.090~5.360、0.110~6.560、0.009~0.534、0.020~1.248、0.391~25.000和0.800~50.800?g/ml范围内线性关系良好。平均加样回收率为93.6%~105.3%,RSD为2.6%~4.3%。
A high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS) method was developed for the simultaneous determination of hydrochlorothiazide (1), nimesulide (2), tetrandrine (3), rutin (4) (5), clozapine (6) and promethazine (7). Acquity UPLC HSS C18 was used as a mobile phase with gradient elution with water: methanol (both containing 0.01% formic acid). Using multiple reaction monitoring, combined with positive and negative ion segmentation scanning. 2,3,6,7 positive mode, 1,4,5 negative mode. 1 to 7 have good linearity in the range of 0.770 ~ 48.650,0.090 ~ 5.360,0.110 ~ 6.560,0.009 ~ 0.534,0.020 ~ 1.248,0.391 ~ 25.000 and 0.800 ~ 50.800 ~ g / ml, respectively. The average recovery was 93.6% ~ 105.3%, RSD was 2.6% ~ 4.3%.