目的 建立菠萝蛋白酶中伏马毒素B₁、B₂、B₃和赭曲霉毒素A的LC-MS/MS法定量分析。方法 采用Phenomenex Kinetex^® C₁₈色谱柱（100 mm×2.1 mm，2.6 μm）；以0.2%甲酸溶液–甲醇为流动相，梯度洗脱，体积流量：0.3 mL/min，柱温：40 ℃，进样体积：5 μL。采用电喷雾离子源（ESI），采集模式为多反应检测（MRM）正离子模式，毛细管电压：3.0 kV；干燥器温度250 ℃，鞘气温度350 ℃，干燥气流量7.0 L/min，雾化气压力30.0 psi，鞘气流量11.0 L/min。结果 伏马毒素B₁、B₂、B₃和赭曲霉毒素A分别在2.0～50.0、1.0～50.0、1.0～50.0、0.5～10.0 μg/kg线性关系良好；平均回收率分别为98.3%、96.8%、102.6%、99.0%，RSD值分别为2.7%、2.7%、2.8%、2.8%。结论 方法具有良好的专属性、线性、精密度，准确度符合要求，可为菠萝蛋白酶的质量控制和标准建立提供依据。

Objective To establish an LC-MS/MS method for the quantitative analysis of fumonisin B₁, B₂, B₃, and ochratoxin A in bromelain. Methods The Phenomenex Kinetex^® C₁₈ column (100 mm × 2.1 mm, 2.6 μm) was used, the mobile phase consisted of 0.2% formic acid solution-methanol, with gradient elution at a flow rate of 0.3 mL/min, column temperature of 40 ℃, and an injection volume of 5 μL. Electrospray ionization (ESI) source was used, operating in positive ion mode with multiple reaction monitoring (MRM). The capillary voltage was set at 3.0 kV, the dryer temperature was 250 ℃, nebulizer gas temperature was 350 ℃, dry gas flow rate was 7.0 L/min, nebulizer gas pressure was 30.0 psi, and nebulizer gas flow rate was 11.0 L/min. Results Fumonisins B₁, B₂, and B₃, as well as ochratoxin A, showed good linear relationships in the ranges of 2.0 — 50.0, 1.0 — 50.0, 1.0 — 50.0, and 0.5 — 10.0 μg/kg, respectively. Their average recovery rates were 98.3%, 96.8%, 102.6%, and 99.0%, with the RSD values of 2.7%, 2.7%, 2.8%, and 2.8%, respectively. Conclusion The method has good specificity, linearity, precision, and accuracy that meets the requirements, which can provide a basis for quality control and standard establishment of bromelain.

R927.2

2025 年国家药品抽检项目（国药监药管[2025]1 号）