不同炮制方法对浙贝母药材3种生物碱含量的影响

Effects of Different Processing Methods on the Contents of 3 Alkaloids in Fritillaria Thunbergii Bulbus

关键词:  浙贝母  高效液相色谱-蒸发光散射检测  硫熏  贝母素甲  贝母素乙  贝母辛  中药材炮制

Key words:  Fritillaria Thunbergii Bulbus  HPLC-ELSD  sulfur fumigation  peimine  peiminine  peimisine  Chinese herbal medicine processing

摘要:

目的 建立一种同时测定浙贝母饮片中贝母素甲、贝母素乙和贝母辛含量的方法，并比较不同产地及炮制方法对其含量的影响。方法 Hypersil C₁₈色谱柱（250 mm×4.6 mm，5 μm），柱温为30℃，流动相为乙腈-0.05%三乙胺水溶液，梯度洗脱，流速为1.0 mL·min^-1，采用ELSD检测，漂移管温度55℃，载气40 psi，增益10。结果 3种成分的峰面积对数值与浓度对数值的线性关系良好（R²≥0.999 1），贝母素甲、贝母素乙和贝母辛的平均回收率（n=9）分别为100.1%，100.1%，96.9%；不同炮制方法处理的浙贝母商品以无硫护色组贝母素甲和贝母素乙总含量最高（0.082%~0.24%，平均为0.15%），生晒处理组次之（0.058%~0.23%，平均为0.13%），硫熏处理组又次之（0.032%~0.12%，平均为0.092%），贝壳灰法组含量最低（0.040%~0.12%，平均为0.072%）。结论 所建立的方法简单、准确、重复性好，可作为评价和控制浙贝母饮片质量的依据；不同炮制方法对浙贝母药材3种生物碱含量有影响，硫熏和贝壳灰法处理会降低浙贝母饮片生物碱的含量。

Abstract:

OBJECTIVE To establish a method for simultaneous determination of peimine, peiminine and peimisine in Fritillaria Thunbergii Bulbus, and compare the contents of different origin and processing methods. METHODS Hypersil C₁₈ column(250 mm×4.6 mm, 5 μm) was used, the temperature of column was maintained at 30℃, using acetonitrile(A)-0.05% triethylamine water solution (B) as the mobile phase by gradient elution at the flow rate of 1.0 mL·min^-1. Using ELSD detection and the temperatures of drift tube were maintained at 55℃, the carrier gas flow rate was 40 psi, gain was 10. RESULTS All the constituents showed good linearity(r² ≥ 0.999 6) in the range of the tested concentration. The average recoveries (n=9) of peimine, peiminine and peimisine were 100.1%, 100.1% and 96.9%, respectively. Compared the contents of different origin and processing methods, the content of peimine and peiminine in the non-sulfur-resistant group was the highest(0.082%-0.24%, average 0.15%), followed by raw sun treatment group (0.058%-0.23%, average 0.13%), followed by sulfur fumigation treatment group (0.032%-0.12%, average 0.092%), shell ash group was the lowest (0.040%-0.12%, average 0.072%). CONCLUSION The validated method has the advantages of simplicity, good precision and reliability, allowing the comprehensive quality control of Fritillaria Thunbergii Bulbus. Different processing methods have effects on the content of 3 alkaloids in Fritillaria Thunbergii Bulbus. Sulfur fumigation and shell ash treatment will reduce the content of alkaloid.