GC-MS/MS自动解卷积和多离子反应监测技术在沉香化气片中挥发性成分定性及定量中的应用

Applications of GC-MS/MS automated mass spectral deconvolution and multi reaction monitor qualitative and quantitative analysis of volatile components of Chenxiang Huaqi Tablets

目的利用气相色谱-串联三重四级杆质谱(GC-MS/MS)结合自动解卷积技术对沉香化气片中挥发性成分进行分析筛查并采用多离子反应监测技术(MRM)建立沉香化气片中多种成分(樟脑、乙酸龙脑酯、百秋李醇)含量测定的方法。方法采用HP-5MS色谱柱(30 m×0.32 mm,0.25μm);升温程序:初始温度100℃,以15℃/min升温至300℃,保持2 min;进样口温度280℃;电离方式:EI离子源(70 e V),离子源温度230℃;四级杆温度150℃;接口温度280℃;进样量为1μL。结果使用解卷积软件共筛选出13个成分,在设定的MRM条件下樟脑、乙酸龙脑酯、百秋李醇质量浓度分别在4.5~90μg/m L(r=0.999 8)、3.3~66μg/m L(r=0.999 8)、2.6~51.5μg/m L(r=0.999 9)与其峰面积的比值呈良好的线性关系;平均回收率(n=6)分别为101.15%、102.64%、100.10%;10批样品樟脑、乙酸龙脑酯、百秋李醇质量分数分别在0.278~0.311、0.381~0.438、0.229~0.381 mg/g。结论该方法准确、简便,重复性好,可用于同时测定沉香化气片中樟脑、乙酸龙脑酯、百秋李醇的含量并为该品种质量的提高提供了参考依据。

Objective To analytically screen the volatile components from Chenxiang Huaqi Tablets（CHT） using gas chromatography-triple quadrupole mass spectrometry（GC-MS/MS） combined with automated mass spectral deconvolution, and establish the methods of multiple components contents（camphor, bornyl acetate, and patchouli alcohol） from CHT using multi reaction monitor（MRM）. Methods The chromatographic column was HP-5 MS（30 m × 0.32 mm × 0.25 μm）. Temperature program： the initial temperature was 100 ℃, at 15 ℃/min up to 300 ℃ for 2 min. Injection port temperature was 280 ℃; Ionization methods： EI ion source with ion source temperature of 230 ℃; Quadrupole temperature was 150 ℃; Interface temperature was 280 ℃; Inject volume was 1 μl. Results A total of thirteen components were screened by automated mass spectral deconvolution soft. Under the conditions of MRM collection, camphor, bornyl acetate, and patchouli alcohol were in the range of 4.5—90 mg/m L（r = 0.999 8）, 3.3—66 mg/m L（r = 0.999 8）, and 2.6—51.5 mg/m L（r = 0.999 9）, respectively, the ratio of each component concentration to its peak area was linear, and the average recovery（n = 6） was 101.15%, 102.64%, and 100.10% respectively; The mass fraction of 10 batches of samples were in the ranges of 0.278—0.311, 0.381—0.438, and 0.229—0.381. Conclusion The method is accurate, simple, and good repeatability. It can be used for the simultaneous determination of camphor, bornyl acetate, and patchouli alcohol in CHT, which provides a reference for the improvement of the quality of this variety.