Objective: To establish a combination method of high performance liquid phase chromatography with UV detector and electrospray detector (HPLC-DAD-CAD) for quantitative screening of 14 additive components including 6 sweeteners and 8 preservatives in Qingrejiedu oral liquid. Methods: The oral solution sample was diluted with water and filtered with a membrane filter, using a Waters XBridge Shield RP18 column (250 mm×4.6 mm, 5 μm). The mobile phase was methanol-20 mmol·L-1 ammonium acetate water with gradient elution. The flow rate was 0.8 mL·min-1, and the column temperature was 35 ℃. Detection wavelengths of DAD detector were 230 nm and 255 nm, and full wavelength detection was turned on at the same time. Acquisition frequency of CAD electrospray detector was 10 Hz with filter of 1 s and atomizer temperature of 35 ℃. Results: The concentration of 14 compounds had good linearity in the range of 0.000 9-0.611 2 mg·mL-1, the correlation coefficients were 0.999 0-1.000, the average recoveries were 91.2%-101.9%, and the RSDs were all below 5.0%. The method was used to screen 200 batches of oral liquid samples involving 44 companies. As a result, benzoic acid and sorbic acid were detected, and saccharin sodium and acesulfame potassium were detected. The contents of benzoic acid in 2 batches of samples from 1 company exceeded the pharmacopoeia standard limit, saccharin sodium in 15 batches of samples from 5 companies, and acesulfame potassium in 4 batches of samples from 2 companies exceeded the proposed limit. Conclusion: The method is simple to operate, highly sensitive, and has good practicability. It can simultaneously screen 14 limited components in oral liquid.
WANG Ya-qiong, ZHONG Shui-sheng, ZHOU Zheng-yu, QIAN Yan, XU Qi, WANG Ming-zhi, ZHANG Chao, CHEN Wei, XUE Man
. Quantitative screening of 14 additive components in Qingrejiedu oral liquid by HPLC-DAD-CAD*[J]. Chinese Journal of Pharmaceutical Analysis, 2022
, 42(12)
: 2136
-2144
.
DOI: 10.16155/j.0254-1793.2022.12.10
[1] 赵立新, 罗标, 刘颖, 等.七省市药用辅料使用管理情况调研报告[J].中国药事, 2014, 28(9):934
ZHAO LX, LUO B, LIU Y, et al. A survey on use and management of pharmaceutical excipients in seven provinces[J].Chin Pharm Aff, 2014, 28(9):934
[2] 刘刚, 雷激, 钟红霞, 等.高效液相色谱蒸发光散射法测定白酒中8种甜味剂的研究[J].食品科技, 2017, 42(7):300
LIU G, LEI J, ZHONG HX, et al. Determination of eight sweeteners in distilled spirits by HPLC evaporative light scattering detector[J].Food Sci Technol, 2017, 42(7):300
[3] 李小亭, 于趁, 谢飞, 等. HPLC-ELSD法同时测定饮料中四种高倍甜味剂的含量[J].中国食品添加剂, 2010(6):217.
LI XT, YU C, XIE F, et al. Determination of four sweeteners in beverage by HPLC-ELSD[J].Chin Food Addit, 2010(6):217
[4] 辜慧, 李道霞, 何成军, 等.高效液相色谱法测定口服液体制剂中12种添加剂的含量[J].中南药学, 2021, 19(7):1411
GU H, LI DX, HE CJ, et al. Determination of 12 additives in oral liquid preparations by HPLC[J].Cent South Pharm, 2021, 19(7):1411
[5] 王亚琼, 张华锋, 周坚.HPLC-CAD法测定中成药中甜味剂及其蜂蜜类辅料的质量评价[J].中成药, 2020, 42(11):3087
WANG YQ, ZHANG HF, ZHOU J. Quality evaluation of sweeteners and honey excipients in chinese patent medicines by HPLC-CAD method[J].Chin Tradit Patent Med, 2020, 42(11):3087
[6] 周凌, 姜范成, 李宪刚, 等.HPLC法同时测定通脉口服液中9种甜味剂和防腐剂的研究[J].中国药物评价, 2019, 36(1):37
ZHOU L, JIANG FC, LI XG, et al. Simultaneous determination of nine sweeteners and preservatives in tongmai oral liquid by HPLC[J].Chin Durg Eval, 2019, 36(1):37
[7] 吴镁春, 吴崇乐.超高效液相色谱法检测两种口服液中糖精钠含量[J].怀化学院学报, 2018, 37(11):74
WU MC, WU CL. Determination of saccharin sodium content in two oral liquids by ultra performance liquid chromatography[J].J Huaihua Univ, 2018, 37(11):74
[8] 李薇, 金薇, 乐健, 等.梯度洗脱HPLC法测定盐酸氨溴索口服溶液中甜味剂含量[J].药物分析杂志, 2012, 32(12):2208.
LI W, JIN W, LE J, et al. Gradient HPLC determination of sweeteners in ambroxol hydrochloride oral solution[J].Chin J Pharm Anal, 2012, 32(12):2208
[9] 俞小娟, 于传飞, 王兰.高效液相色谱-电喷雾法测定单克隆抗体药物中海藻糖的含量[J].药物分析杂志, 2021, 41(10):1729
YU XJ, YU CF, WANG L. Development of an HPLC-CAD method to determine trehalose in therapeutic monoclonal antibody[J].Chin J Pharm Anal, 2021, 41(10):1729.
[10] 张伟, 张慧, 梁成罡.HPLC-CAD法测定壬苯醇醚及壬苯醇醚栓中游离PEG的含量[J].药物分析杂志, 2021, 41(8):1417
ZHANG W, ZHANG H, LIANG CG.Determination of free PEG in nonoxinol and nonoxinol suppositories by HPLC-CAD[J].Chin J Pharm Anal, 2021, 41(8):1417
[11] 南易, 郑伟, 马凤霞, 等.HPLC-CAD同时测定知母中芒果苷和知母皂苷BⅡ的含量[J].药物分析杂志, 2021, 41(1):111
NAN Y, ZHENG W, MA FX, et al. Simultaneous determination of mangiferin and timosaponin BⅡ of Anemarrhenae Rhizoma by HPLC-CAD[J].Chin J Pharm Anal, 2021, 41(1):111
[12] 赵慧.HPLC-CAD法测定阿卡波糖胶囊含量[J].药物分析杂志, 2020, 40(5):910
ZHAO H.Determination of acarbose capsules by HPLC-CAD[J].Chin J Pharm Anal, 2020, 40(5):910
[13] 白钢钢, 袁斐, 叶慧, 等.HPLC-CAD法测定4种银杏叶制剂中萜类内酯类成分的含量[J].药物分析杂志, 2019, 39(6):1102
BAI GG, YUAN F, YE H, et al. Determination of ginkgolides in four kinds of Ginkgo leaf preparations by HPLC-CAD[J].Chin J Pharm Anal, 2019, 39(6):1102
[14] 侯爱荣, 邢晔忠, 吴雪松.HPLC-CAD法同时测定二陈丸中7个活性成分的含量[J].药物分析杂志, 2019, 39(4):662
HOU AR, XING YZ, WU XS.Simultaneous determination of seven active ingredients in Erchen pills by HPLC-CAD[J].Chin J Pharm Anal, 2019, 39(4):662
[15] 孙亚灵, 赵恂, 张玫, 等.蔗糖及其有关物质含量的HPLC-CAD分析研究[J].药物分析杂志, 2019, 39(4):588
SUN YL, ZHAO X, ZHANG M, et al. Determination of sucrose and its related substances by HPLC-CAD[J].Chin J Pharm Anal, 2019, 39(4):588
