GC法测定拟黑多刺蚁中棕榈酸和油酸的含量  

GC determination of palmitic acid and oleic acid in Poryrhaehis vicina Roger

作　　者：刘吉成 韦桂宁[2] 卢文杰[2] 陆国寿[2] 谭晓[2] 黄周锋[2] 陆奇志 

机构地区：[1]广西玉林食品药品检验所,玉林537000 [2]广西中医药研究院,南宁530022 [3]广西江滨医院药剂科,南宁530021

出　　处：《药物分析杂志》2016年第1期86-90,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金(81360653);国家自然科学基金(81560663);广西中医药民族医药继承创新工程课题(GZPT13-29);广西壮族自治区卫生和计划生育委员会中医药科技专项(GZBZ16-09)

摘　　要：目的:建立拟黑多刺蚁中棕榈酸和油酸含量的测定方法。方法:使用氢氧化钾甲醇溶液将拟黑多刺蚁中的脂肪酸甲酯化,采用正十八烷作为内标物,用气相色谱法测定拟黑多刺蚁中棕榈酸和油酸。色谱条件:色谱柱为Rtx~-5毛细管柱(30 m×0.32 mm×0.25μm);柱流量2.0 mL·min^(-1);总流量25.0 mL·min^(-1);柱温采用程序升温方式,80℃保持1 min,15℃·min^(-1)升到220℃保持5 min;FID检测器温度250℃;载气为N_2(30.0 mL·min^(-1)),H_2(40.0 mL·min^(-1)),空气(400.0 mL·min^(-1));进样口温度230℃;进样量1μL,分流进样,分流比为10:1。结果:棕榈酸甲酯进样量在0.039 9~1.597μg范围内呈良好线性关系,回归方程为Y=0.980 8X-0.156 3(r=0.999 4),平均回收率为100.1%(RSD=1.4%);油酸甲酯进样量在0.039 4~1.576μg范围内呈良好线性关系,回归方程为Y=1.103 3X+0.146 7(r=0.999 4),平均回收率为92.4%(RSD=1.5%)。广西横县、桂林、贵港、灵山、上林、都安6个产地的拟黑多刺蚁样品中,棕榈酸的含量分别为20.86、5.34、11.55、22.66、21.61、22.23 mg·g^(-1),油酸的含量分别为48.52、18.62、33.09、53.75、50.36、52.48 mg·g^(-1)。结论:本方法经方法学验证,可用于拟黑多刺蚁中油酸和棕榈酸的含量测定。Objective： To establish a GC method for content determination of palmitic acid and oleic acid in Poryrhaehis vicina Roger. Methods： Palmitic acid and oleic acid were determined by GC method after saponification and methylation, with potassium hydroxide-methanol as methylated reagent and octadecane as internal standard. The chromatographic condition was as follows ： Rtx-5 restek capillary column （ 30 m × 0.32 mm × 0.25 μm ） was adopted ; Pillars flow was 2.0 mL· min^-1, and total flow was 25.0 mL·min^-1. Column temperature was first kept at 80 ~C for 1 min, and then raised to 220 ℃ with rate of 15 ℃ · min^-1 and maintained for 5 min; FID was used as detector and the temperature was 250 ℃ ; nitrogen （ 30.0 mL·min^-1 ）, hydrogen （ 40.0 mL·min^-1 ）and air （ 400.0 mL· min^-1 ）were used as carrier was; iniection port temperature was 230℃ ;sample size was 1 μ L; split injection and diversion ratio was 10 ： 1. Results： Methyl palmitate had good linear relationship in the range of 0.039 9-1.597μ g, the regression equation was Y=0.980 8X-0.156 3 （ r=0.999 4 ） , the average recovery was 100.1% with RSD of 1.4%; methyl oleate had good linear relationship in the range of 0.039 4-1.576 Ix g, the regression equation was Y=l.103 3X ＋ 0.146 7 （ r=0.999 4 ）, the average recovery was 92.4% with RSD of 1.5%. The contents of palmitic acid in Poryrhaehis vicirta Roger of six origin such as Hengxian, Guilin, Guigang, Lingshan, Shanglin and Du＇ an were 20.86, 5.34, 11.55,22.66, 21.61, and 22.23 mg·g^-1, and the contents of oleie acid were 48.52, 18.62, 33.09, 53.75,50.36 and 52.48 mg·g^-1, respectively. Conclusion： The method established in this paper conforms to the requirements of the methodology validation, and thus can be used for quality control of fatty acid of Poryrhaehis vicina Roger.

关 键 词：拟黑多刺蚁 气相色谱法 棕榈酸 油酸 动物药含量测定 

分 类 号：R917[医药卫生—药物分析学]