建立了乳制品中3种β-内酰胺酶抑制剂克拉维酸钾、他唑巴坦和舒巴坦的提取和固相萃取净化方法.样品经水溶后,用丙酮沉淀蛋白质.上清液在弱酸性条件下用PWAX固相萃取小柱(60 mg/3 mL)富集、净化,0.05％(如无特殊说明均为体积分数)氨水-甲醇溶液洗脱.然后采用高效液相色谱-二极管阵列检测器(HPLC-PAD)分离检测.分析柱为资生堂CAPCELL PAK MG-C18(150 mm× 4.6 mm,5μm)；流动相为0.03％磷酸-乙腈.该方法对克拉维酸钾、他唑巴坦和舒巴坦的最低检测质量浓度均为0.03 mg/L；纯牛奶、酸奶和奶粉中的回收率在84.6％～101.7％之间,RSD在2.2％～7.4％之间(n=6)；在0.05～5 mg/L范围内均呈良好的线性关系,线性回归系数r＞0.999.该方法的前处理净化效果好、检测灵敏度高、回收率和重现性良好,适用于乳制品中β-内酰胺酶抑制剂的测定.
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