高效液相色谱法同时测定明胶空心胶囊中苯甲酸和山梨酸  

Simultaneous determination of benzoic acid and sorbic acid in vacant gelatin capsules by high performance liquid chromatography

作　　者：刘康连 梁晓玲 黎强 樊文研 庞云娟 陈宇 LIU Kanglian;LIANG Xiaoling;LI Qiang;FAN Wenyan;PANG Yunjuan;CHEN Yu(YuLin Food and Drug Inspection and Testing Center,Yulin Engineering and Technology Center for Quality Detection and evaluation of Chinese medicinal materials(including spices),Yulin 537000,China)

机构地区：[1]玉林市食品药品检验检测中心,玉林中药材(含香辛料)质量检测与评价工程技术中心,广西玉林537000

出　　处：《化学分析计量》2024年第1期46-52,共7页Chemical Analysis And Meterage

基　　金：广西科技基地和人才专项(桂科AD22080002);广西科技重大专项(桂科AA23023035)。

摘　　要：建立明胶空心胶囊中苯甲酸、山梨酸的高效液相色谱测定方法。样品经水浴溶解,加入蛋白质沉淀剂并结合C18固相萃取小柱去除蛋白质,用体积分数为60%甲醇水溶液洗脱,定容后过0.45μm滤膜,以Agilent Zorbax SB-Aq色谱柱(250 mm×4.6 mm,5μm)为分析柱,以2 mmol/L甲酸与20 mmol/L乙酸铵混合溶液-甲醇(体积比为90∶10)为流动相,流量为1.0 mL/min,检测波长为230 nm。苯甲酸、山梨酸的质量浓度在0~50 mg/L范围内与色谱峰面积线性良好,相关系数分别为0.9998和0.9999,方法检出限分别为3、4 mg/kg,定量限分别为6、9 mg/kg。测定结果的相对标准偏差为1.9%、2.2%(n=6),样品加标平均回收率为92.4%~106.1%。该方法操作简便,灵敏度高,稳定性良好,可用于明胶空心胶囊中苯甲酸及其钠盐(以苯甲酸计)、山梨酸及其钾盐(以山梨酸计)的同时测定。A method for the determination of benzoic acid and sorbic acid in vacant gelatin capsules by high performance liquid chromatography was established.The samples were dissolved in water bath,protein precipitant was added and combined with C18 solid phase extraction column to remove the protein.The protein was eluted with 60%volume fraction methanol aqueous solution,and after constant volume,it was filtered with 0.45μm filter membrane.Agilent Zorbax SB Aq chromatographic column(250 mm×4.6 mm,5μm)was used as analytical column.The mixed solution of 2 mmol/L formic acids with 20 mmol/L ammonium acetate-methanol(volume ratio was 90∶10)was used as the mobile phase,and the flow rate was 1.0 mL/min.The detection wavelength was 230 nm.The mass concentration of benzoic acid and sorbic acid had a good linear relationship with the chromatographic peak area in the range of 0-50 mg/L,the correlation cofficients were 0.9998 and 0.9999,respectively.The detection limits were 3 mg/kg and 4 mg/kg,and the quantitative limits were 6 mg/kg and 9 mg/kg,respectively.The relative standard deviations of the determination results were 1.9%and 2.2%(n=6),respectively.The average recovery rates of the sample spiked were 92.4%-106.1%.This method is easy to operate,highly sensitive,and has good stability,which can be used for simultaneous determination of benzoic acid and its sodium salt(calculated by benzoic acid),sorbic acid and its potassium salt(calculated by sorbic acid)in vacant gelatin capsules.

关 键 词：高效液相色谱法 明胶空心胶囊 防腐剂 苯甲酸 山梨酸 

分 类 号：O657.7[理学—分析化学]