UPLC-DAD快速筛查抗风湿类保健食品及中成药中非法添加的19个化学物质

Rapid determination of illegally added chemical drugs in anti-rheumatic Chinese traditional patent medicine and health foods by UPLC-DAD

目的:建立快速检测抗风湿类中成药及保健食品中典型的19个非法添加的化学物质的分析方法。方法:采用甲醇超声提取样品中的抗风湿类化学物质,并应用超高效液相色谱-二极管阵列检测器法(UPLCDAD)测定其含量。色谱条件:采用Luna UPLC C18色谱柱(2.1 mm×100 mm,1.6μm),以20 mmol·L^-1醋酸铵水溶液(含0.01%三乙胺)-乙腈为流动相进行梯度洗脱,流速为0.3 mL·min^-1,柱温为35℃,检测波长为230 nm,对19个抗风湿类化学物质进行定性、定量检测。结果:19个化学物质在相应的浓度范围内与其对应峰面积呈良好的线性关系,相关系数均大于0.999 9。液体样品平均回收率为98.1%~99.5%,RSD为0.40%~1.1%;固体样品平均回收率为98.3%~100.4%,RSD为1.4%~2.3%。应用该方法对10批次样品进行检测,共有5批检出阳性,其中3批检出醋酸泼尼松、布洛芬、吲哚美辛、吡罗昔康、双氯芬酸钠;2批检出对乙酰氨基酚。并采用超高效液相色谱-质谱联用法进一步确证。结论:本方法操作简便,精密度、稳定性、重复性好,能够达到快速检验抗风湿类中成药及保健食品中非法添加化学成分的目的。

Objective:To develop a method for determination of 19 illegal addition of the typical chemicals in anti-rheumatic traditional Chinese medicine and health foods. Methods:The samples were extracted by ultrasonic machine with methanol and the content were determined by UPLC(DAD).The separation was performed on Luna UPLC C18 column(2.1 mm×100 mm,1.6 μm) with 20 mmol·L^-1 ammonium acetate solution(containing 0.01% triethylamine) and acefonifrile as the moblie phase by gradient elution at the flow rate of 0.3 mL·min^-1,and column temperature was 35 ℃. The detection wavelength was set at 230 nm for qualification and quantification. Results:The calibration curves were linear within the ranges of corresponding concentration. The correlation coefficients were above 0.999 9. The average recoveries of the liquid sample were 98.1%-99.5% with RSDs within 0.4%-1.1%. The average recoveries of the solid sample were 98.3%-100.4% with RSDs within 1.4%-2.3%. 5 batches of positive samples were detected in 10 batches of samples. Prednisone acetate,ibuprofen,indometacin,piroxicam and diclofenac sodium were detected in three batches. Paracetamol was found in two batches. The samples were further confirmed by UPLC-MS/MS. Conclusion:The established method is simple,accurate,stable and reproducible,and can be used for simultaneous determination of 19 illegally added into anti-rheumatic traditional Chinese medicine and health foods.