高效液相色谱法同时测定生脉饮中9种抑菌剂含量

Simultaneous Determination of Nine Bacteriostatic Agents in Shengmai Drink by HPLC

目的 建立同时测定生脉饮中9种抑菌剂含量的高效液相色谱法,并考察该制剂抑菌剂添加情况。方法 色谱柱为Shiseido Capcell Pak MGⅡC18柱(250 mm×4.6 mm,5μm),流动相为0.02 moL/L乙酸铵溶液-甲醇(梯度洗脱),流速为1.0 mL/min,检测波长为230 nm(苯甲酸)、254 nm(山梨酸钾、羟苯甲酯、羟苯乙酯、羟苯丙酯、羟苯丁酯、4-羟基苯甲酸异丁酯、4-羟基苯甲酸戊酯、4-羟基苯甲酸苯酯),柱温为30℃,进样量为20μL。选取16家生产企业38批次样品(均为2022年江苏省评价性抽验样品),按不同倍数稀释后检测9种抑菌剂含量。结果 9个待测成分进样量分别在0.011~1.062μg,0.010~1.001μg,0.010~0.971μg,0.011~1.047μg,0.010~0.956μg,0.010~1.039μg,0.010~0.958μg,0.011~1.108μg,0.010~1.032μg范围内与峰面积线性关系良好(r≥0.998 3);精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率为91.47%~97.16%,RSD为0.15%~1.24%(n=6)。16家生产企业38批次产品中个别存在添加处方外抑菌剂、超标准限量添加抑菌剂的情况。结论 该方法准确性、专属性良好,可用于生脉饮中抑菌剂的测定。

Objective To establish a high-performance liquid chromatography(HPLC)method for simultaneously determining the contents of nine bacteriostatic agents in Shengmai Drink,and to investigate the addition of bacteriostatic agents in the formulation.Methods The chromatographic column was the Shiseido Capcell Pak MGⅡC18 column(250 mm×4.6 mm,5μm),the mobile phase was 0.02 mol/L ammonium acetate solution-methanol(gradient elution),the flow rate was 1.0 mL/min,and the detection wavelengths were 230 nm(benzoic acid)and 254 nm(potassium sorbate,methylparaben,ethylparaben,propylparaben,butylparaben,isobutyl 4-hydroxybenzoate,pentyl 4-hydroxybenzoate,phenyl 4-hydroxybenzoate),the column temperature was 30℃,and the injection volume was 20μL.Thirty-eight batches of samples from 16 manufacturing enterprises(all of which were evaluative samples in Jiangsu in 2022)were selected and diluted at different proportions,and the contents of nine bacteriostatic agents were determined.Results The linear ranges of the nine components to be tested were 0.011-1.062μg,0.010-1.001μg,0.010-0.971μg,0.011-1.047μg,0.010-0.956μg,0.010-1.039μg,0.010-0.958μg,0.011-1.108μg,0.010-1.032μg(r≥0.9983),respectively.The RSDs of precision,stability and repeatability tests were all lower than 2.0%.The average recovery rates of the above nine components were in the range of 91.47%-97.16%,with RSDs in the range of 0.15%-1.24%(n=6).Among the 38 batches of samples from 16 manufacturing enterprises,there were few cases of adding bacteriostatic agents not included in the prescription or over the standard limit.Conclusion This method is accurate and specific,which can be used for the determination of bacteriostatic agents in Shengmai Drink.