RP-HPLC法测定热感赛比斯坦颗粒中3种生物碱成分的含量  

Determination of 3 alkaloids in Regan Saibisitan granules by RP-HPLC method

作　　者：刘新豫 司晓萍 唐辉[1] 庞克坚 翟欣[1] 孙小雅[1] 王亚乔 

机构地区：[1]新疆特种植物药资源教育部重点实验室,石河子大学药学院,石河子832002 [2]新疆第八师石河子市药品检验所,石河子832000 [3]和田维吾尔药业有限责任公司,和田848200

出　　处：《药物分析杂志》2017年第5期897-902,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金(81260627);八师石河子市科技计划项目(2016HZ32)

摘　　要：目的:建立热感赛比斯坦颗粒中吗啡、可待因和罂粟碱3种生物碱成分的含量测定方法。方法:采用高效液相法进行定量分析。吗啡含量测定选用C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.01 mol·L^(-1)磷酸二氢钾和0.05 mol·L^(-1)庚烷磺酸钠混合水溶液(pH 3.1)(2∶98)为流动相,流速1 mL·min^(-1),检测波长220 nm;柱温28℃。可待因和罂粟碱含量测定选用C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈(A)-0.01 mol·L^(-1)磷酸二氢钾和0.05 mol·L^(-1)庚烷磺酸钠混合水溶液(pH 3.8)(B)为流动相进行梯度洗脱(0~18 min,2%A→40%A;18~25 min,40%A→52%A),流速1 mL·min^(-1),检测波长分别为220 nm和257 nm,柱温28℃。结果:吗啡、磷酸可待因和盐酸罂粟碱进样量分别在0.119~23.760、0.057~3.983和0.022~3.906μg范围内,与峰面积线性关系良好(r=0.999 2~0.999 9),平均回收率(n=6)分别为100.2%、100.0%和100.2%。3批样品中吗啡、可待因和罂粟碱的含量分别为0.030~0.031、0.440~0.444和0.011~0.012 mg·g^(-1)。结论:该方法可用于热感赛比斯坦颗粒中3种生物碱的含量测定。Objective： To establish the method for determination of morphine, codeine and papaverine in Regan Saibisitan granules. Methods： High performance liquid chromatography method was employed for the analyses of three alkaloids in Regan Saibisitan granules. Morphine analysis was carried out on C18 column （ 250 mm × 4.6 mm, 5 μm ） with mobile phase consisting of acetonitrile-0.01 mol· L^-1 monopotassium phosphate and 0.05 mol· L^-1 sodium heptanesulfonate solution （pH 3.1 ） （2：98）. The flow rate was 1.0 mL· min^-1 and the detection wavelength was 220 nm. The column temperature was maintained at 28 %. Analyses of codeine and papaverine were carried out on C18 column （ 250 mm × 4.6 mm, 5 μm ） with mobile phase consisting of acetonitrile （ A ） -0.01 mol· L^-1 monopotassium phosphate and 0.05 mol· L^-1 sodium heptanesulfonate solution （ pH 3.8 ） （ B ） by gradient elution （ 0-18 min, 2%A → 40%A; 18-25 min, 40%A → 52%A ）. The flow rate was 1.0 mL· min^ -1 and the detection wavelengths were 220 nm and 257 nm. The column temperature was maintained at 28 ℃. Results： The linear ranges of morphine, codeine phosphate and papaverine hydrochloride were 0.119-23.760 μg （ r=0.999 8 ）, 0.057-3.983 μg （ r=0.999 9 ） and 0.022-3.906 μg （ r=0.999 2 ）, respectively. The average recoveries （tt=6）were 100.2%, 100.0% and 100.2%, respectively. The contents of morphine, codeine and papaverine in 3 samples were 0.030-0.031 mg· g^-1,0.440-0.444 mg· g^-1and 0.011-0.012 mg· g^-1 , respectively. Conclusion： The established determination method is proved by methodology validation that it can be used for the detection of 3 alkaloids of opium poppy shell and seed in Regan Saibisitan granules.

关 键 词：维吾尔药 感冒验方 民族药 热感赛比斯坦颗粒 罂粟壳 生物碱 吗啡 可待因 罂粟碱 高效液相色谱 

分 类 号：R917[医药卫生—药物分析学]