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

Rapid and Simultaneous Analysis of 11 Adulterated Drugs in Herbal Tea by HPLC

采用核-壳亚3μm色谱柱建立了高效液相色谱同时测定凉茶中11种非法添加药物（对乙酰氨基酚、阿司匹林及其降解物水杨酸、磺胺甲唑、磺胺嘧啶、磺胺二甲嘧啶、氧氟沙星、环丙沙星、洛美沙星、土霉素、强力霉素）的方法。样品经甲醇-乙腈（1∶1）超声提取,安捷伦Poroshell 120 EC C18（100 mm×4.6mm,2.7μm）色谱柱分离,以0.1%三氟乙酸三乙胺溶液（pH 3.0）-甲醇-乙腈为流动相,梯度洗脱,流速1.2 mL/min,柱温35℃,采用二极管阵列检测器检测,外标法定量。11种成分的线性范围为0.5-25 mg/L,相关系数均不小于0.998 2,检出限为1-5 mg/L,平均回收率为86.9%-108.0%,相对标准偏差（RSD）为0.5%-1.4%。按上述方法对286批凉茶样品进行检测,发现9批阳性样品,检出成分为对乙酰氨基酚、阿司匹林及其水解物水杨酸、磺胺甲唑。阳性样品进一步采用液质联用法定性确证。该方法操作简便、灵敏、准确,适用于凉茶中11种化学成分的测定。

A high performance liquid chromatographic（ HPLC） method for the determination of 11 adulterated drugs（ acetaminophen,aspirin,salicylic acid, sulfapirazinmetossina, sulfadiazine,sulfamethazine, ofloxacin,ciprofloxacin, lomefloxacin, terramycin and doxycycline） in herbal tea was developed. The samples were extracted ultrasonically with methanol- acetonitrile（ 1 ∶ 1）,and the extracts were separated on an Agilent Poroshell 120 EC C18column（ 100 mm × 4. 6 mm,2. 7 μm）with trifluoroacetic acid triethylamine（ pH 3. 0）- methanol- acetonitrile as mobile phases by gradient elution. The flow rate was 1. 2 mL / min and the column temperature was 35 ℃. Identification of 11 compounds was achieved by the comparison of the chromatographic peaks ＇ retention times and the DAD spectra between the samples and reference substances. Quantification analysis was performed by the external standard method. The calibration curves showed good linearities in the range of 0. 5- 25 mg / L with correlation coefficients not less than 0. 998 2. The detection limits of 11 compounds ranged from 1 mg / L to 5 mg / L. The average recoveries ranged from 86. 9% to 108. 0% with RSDs of 0. 5%- 1. 4%. The method was applied in the analysis of 286 herbal tea samples,and 9 positive samples containing acetaminophen,aspirin,salicylic acid and sulfapirazinmetossina were found. The positive samples were further identified and verified by HPLC- MS / MS. The experimental results indicated that the proposed method was simple,sensitive and accurate,and was suitable for the determination of 11 adulterated drugs in herbal tea.