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目的采用液质联用法同时测定骨头帮胶囊中非法添加的吡罗昔康、醋酸泼尼松、双氯芬酸钠和布洛芬。方法采用Kromasil C18色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-20 mmol.L-1乙酸铵溶液(0.1%乙酸)(43∶57),测定波长为330、240、280、220 nm,流速0.8 mL.min-1,柱温45℃。离子源为ESI源,正、负离子模式进行定性检测,采用HPLC法测定含量。结果在HPLC-MS/MS中,受试制剂中分别检测出与吡罗昔康、醋酸泼尼松、双氯芬酸钠及布洛芬对照品一致的色谱峰、质谱峰。结论所用方法选择性强、灵敏度好,结果准确可靠,可作为检测骨头帮胶囊中违禁添加吡罗昔康、醋酸泼尼松、双氯芬酸钠及布洛芬的有效方法。
OBJECTIVE: To simultaneously determine piroxicam, prednisone acetate, diclofenac sodium and ibuprofen illegally added in Bone Granule Capsules by liquid chromatography-mass spectrometry. Methods A Kromasil C18 column (250 mm × 4.6 mm, 5 μm) was used with a mobile phase of acetonitrile-20 mmol·L-1 ammonium acetate (0.1% acetic acid) (43:57) 220 nm, flow rate 0.8 mL.min-1, the column temperature 45 ℃. The ion source was ESI source, positive and negative ion modes were qualitatively detected, and the content was determined by HPLC. Results In HPLC-MS / MS, the peaks of the chromatograms and the peaks of the mass spectrometry peaks corresponding to the reference standard of piroxicam, prednisone acetate, diclofenac sodium and ibuprofen were respectively detected in the test preparations. Conclusion The method used is selective, sensitive and reliable. It can be used as an effective method to detect piroxicam, prednisone acetate, diclofenac sodium and ibuprofen banned in bone-in-capsule.