气相色谱法同时测定复方丹参片中樟脑残留量及冰片含量

Simultaneous Determination of Residual Camphor and Borneolum in Compound Danshen Tablets by Gas Chromatography

目的建立同时测定复方丹参片中樟脑残留量及冰片含量的气相色谱法。方法色谱柱为Agilent17903-113I聚乙二醇-20m毛细管色谱柱(30m×0.25mm,0.25μm),温度进样口为220℃、气化室为250℃、氢火焰离子化检测器为250℃,流速载气高纯度氮气为3mL/min、氢气为40mL/min、空气为400mL/min,尾吹为35mL/min、柱温程序升温(初始温度为100℃,保持5min,以10℃/min的速率升温至110℃,保持5min,再以相同速率升温至160℃,保持4min),分流比为5∶1。结果樟脑、龙脑和异龙脑的质量浓度线性范围分别为4.513~56.407μg/mL(r=0.9998),13.932~174.151μg/mL(r=0.9997),9.098~113.719μg/mL(r=0.9996);精密度、稳定性、重复性试验结果的RSD均小于2%;回收率分别为98.88%,99.23%,93.93%(RSD分别为0.88%,0.33%,0.10%)。结论该方法简便、快速、准确、重复性好,可用于复方丹参片的质量控制。

Objective To establish a gas chromatography for simultaneous determination of residual camphor and borneolum in Compound Danshen Tablets. Methods The chromatographic column was Agilent 17903-113 I polyethylene glycol-20 m capillary column( 30 m ×0. 25 mm,0. 25 μm),the temperature was 220 ℃ for inlet,250 ℃ for gasification chamber,250 ℃ for flame ionization detector,the flow rate of carrier gas was 3 mL/min for high purity nitrogen,40 mL/min for hydrogen,400 mL/min for air and 35 mL/min for tail gas. The temperature-programmed was adopted for column temperature( the initial temperature was 100 ℃,maintained for 5 min,the temperature was raised to 110 ℃ at the rate of 10 ℃/min,maintained for 5 min,and then it was raised to 160 ℃ at the same rate,maintained for 4 min). The split ratio was 5 ∶ 1. Results Camphor,borneol and isoborneol showed good linear relationship with peak area in the ranges of 4. 513-56. 407 μg/mL( r = 0. 999 8),13. 932-174. 151 μg/mL( r = 0. 999 7) and 9. 098-113. 719 μg/mL( r = 0. 999 6). RSDs of precision,stability and repeatability test results were less than 2%. The recoveries were 98. 88%,99. 23% and93. 93% and RSDs were 0. 88%,0. 33% and 0. 10%,respectively. Conclusion The method is simple,rapid,accurate and reproducible,which can be used for the quality control of Compound Danshen Tablets.