作者：温家欣1, 曹雅静1, 何嘉雯1, 钟常风2, 赖宇红1
作者单位：1. 广东省药品检验所, 广东 广州 510663;
2. 广州新华学院, 广东 广州 510520
关键词：凉茶;非法添加;抗病毒类药物;镇咳祛痰类药物;抗组胺类药物
摘要：
文章以临床常用、与感冒咳嗽适应症高度吻合的8种化学药物为研究对象，建立高效液相色谱-串联质谱同时测定多种非法添加化学药物的分析方法。样品经甲醇超声提取，以5 mmol/l甲酸铵溶液（含0.1%甲酸）–0.1%甲酸乙腈为流动相体系进行梯度洗脱，采用agilent poreshell ec-c18（100 mm×2.1 mm，2.7 μm）色谱柱分离，外标法定量。8种目标化合物在线性范围内线性关系良好，相关系数均大于0.9993，方法检出限为0.01~0.3 mg/kg，方法定量限为0.025~1 mg/kg，基质效应系数的绝对值均小于18%。各目标化合物的平均回收率为65.0%~105.7%，重复性相对标准偏差（n=6）范围为1.6%~10.6%，24 h内进样精密度相对标准偏差均小于6%。该方法简单快速，灵敏度高，准确性、重复性和稳定性良好，填补现行标准的技术空白，可满足实际检验工作的需要。
determination of 8 adulterated drugs in herbal tea by high performance liquid chromatography-tandem mass spectrometry
wen jiaxin1, cao yajing1, he jiawen1, zhong changfeng2, lai yuhong1
1. guangdong institute for drug control, guangzhou 510663, china;
2. guangzhou xinhua college, guangzhou 510520, china
abstract: an analytical method for the simultaneous determination of adulterants by high performance liquid chromatography-tandem mass spectrometry (hplc-ms/ms) was established for 8 kinds of chemical drugs, which were commonly used in clinic and highly consistent with the indications of cold and cough. the samples were extracted by ultrasonic extraction with methanol and eluted by gradient elution using 5 mmol/l ammonium formate solution (containing 0.1% formic acid) –0.1% formic acid acetonitrile as mobile phase system. the separation was performed on an agilent poreshell ec-c18 column (100 mm×2.1 mm, 2.7 μm), and quantified by external standard method. the 8 target compounds showed good linear relationships within their respective linear ranges, with correlation coefficients (r) great than 0.9993. the limits of detection(lods) ranged from 0.01 mg/kg to 0.3 mg/kg, the limits of quantification(loqs) ranged from 0.025 mg/kg to 1 mg/kg, and the absolute values of matrix effect coefficients(mes) were all less than 18%. the average recoveries of the target compounds ranged from 65.0% to 105.7%, and the relative standard deviations(rsds, n=6) of repeatability ranged from 1.6% to 10.6%, and the relative standard deviations of injection precision within 24 h were all less than 6%. the method is simple, rapid, sensitive, accurate, repeatable and stable, which meets the requirements of quantitative analysis and can meet the needs of practical inspection.
keywords: herbal tea;adulteration;antiviral drugs;antitussive and expectorant drugs;antihistamines drugs
2023, 49(6):62-67 收稿日期: 2021-11-15;收到修改稿日期: 2022-01-28
基金项目: 广东省医学科学技术研究基金(b2021300)；广东省药品监督管理局科技创新项目（2022tdz02，sn2022024）
作者简介: 温家欣(1986-),女,广东广州市人,主管药师,硕士,主要从事食品药品检验检测工作
参考文献
[1] 温家欣, 陈林, 赖宇红, 等. 高效液相色谱法同时快速测定凉茶中11种非法添加化学药物[j]. 分析测试学报, 2016, 35(3): 285-291
[2] 尹佳, 黎星, 张涛, 等. 网购凉茶中非法添加抗风湿类药物状况分析及对策探讨[j]. 食品安全质量检测学报, 2018, 9(18): 4964-4970
[3] 梁少东, 刘莉丽, 伍国怡, 等. 超高效液相色谱-串联质谱法测定凉茶中3种非法添加的解热镇痛药物[j]. 食品安全质量检测学报, 2021, 12(10): 3965-3969
[4] 何嘉雯, 温家欣, 赖宇红, 等. 高效液相色谱快速测定草本植物饮料中28种外源性药物和内源性成分[j]. 色谱, 2018, 36(8): 758-765
[5] 罗伟, 杜俊威, 林秋凤, 等. 高效液相色谱-串联质谱法测定凉茶中20种非法添加化学药物[j]. 亚太传统医药, 2020, 16(6): 43-47
[6] 宋宁宁, 张科明, 刘向红, 等. quechers-超高效液相色谱-串联质谱法快速测定凉茶中非法添加的12种化学药物[j]. 色谱, 2015, 33(10): 1026-1031
[7] 唐维英, 黄泽玮, 钱广生, 等. 超高效液相色谱-串联质谱法测定茶叶、代用茶和饮料食品中63种非法添加化合物[j]. 色谱, 2018, 36(12): 1245-1260
[8] 温家欣, 陈林, 杨文杰, 等. 利用核-壳亚3微米填料色谱技术快速测定镇痛类健康产品中25种非法添加药物[j]. 理化检验(化学分册), 2017, 53(6): 621-626
[9] 辜慧, 杜钢, 李澍才, 等. uplc-ms/ms法检测中药制剂中的27种非法添加化药成分[j]. 中国测试, 2021, 47(7): 49-54
[10] 张宏峰, 彭荣飞, 罗晓燕, 等. quechers-超高效液相色谱-串联质谱法测定散装凉茶中非法添加的6种化学药物[j]. 中国卫生检验杂志, 2017, 27(16): 2287-2290
[11] 刘辉, 熊波, 陈磊, 等. 凉茶中对乙酰氨基酚酶联免疫检测方法的研究[j]. 广东化工, 2017, 44(11): 62-63
[12] 宋健. 表面增强拉曼光谱法快速检测中成药中吡罗昔康[j]. 化学分析计量, 2020, 29(2): 49-53
[13] 温海滨, 林洁纯, 叶靖怡, 等. quechers-超高效液相色谱-串联质谱法同时测定水产品中20种苯并咪唑类药物及其代谢物残留[j]. 食品安全质量检测学报, 2021, 12(18): 7214-7221
[14] goulart b v, vizioli b, espindola e, et al. matrix effect challenges to quantify 2, 4-d and fipronil in aquatic systems[j]. environmental monitoring and assessment, 2020, 192: 797-808
[15] 温家欣, 吴凤丹, 曹雅静, 等. 高效液相色谱-串联质谱法测定蜂胶及以其为原料的保健食品中的氯霉素[j]. 色谱, 2018, 36(12): 1284-1289
[16] kaczyński p. clean-up and matrix effect in lc-ms/ms analysis of food of plant origin for high polar herbicides[j]. food chemistry, 2017, 230: 524-531
