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目的利用总有机碳(total organic carbon,TOC)分析仪建立血液制品清洁验证分析方法。方法制备碳浓度为5、10、15 ppm的牛血清白蛋白(bovine serum albumin,BSA)溶液,检测TOC值,并计算回收率,验证方法的准确性;制备6份碳浓度为10 ppm的BSA溶液,检测TOC值,计算相对标准偏差(relative standard deviation,RSD),验证方法的重复性;制备碳浓度分别为0、1、2.5、5、10、15和20 ppm的BSA溶液,检测TOC值,验证方法的线性;测定10次TOC检测用水的TOC值,计算SD,确定方法的检测限(limit of detection,LOD)和定量限(limit of quantitation,LOQ);制备碳浓度分别为0、1、2.5、5、10、15和20 ppm的BSA溶液,先以从低到高浓度,再以从高到低浓度顺序分析,检测TOC值,分别计算回归曲线决定系数,确定残留效应;分别在不锈钢和玻璃材质上擦拭取样,检测TOC值,计算回收率及RSD。对清洁后的血液制品生产用设备和器具擦拭取样,检测TOC值,确认清洁效果。结果 3个碳浓度的BSA溶液TOC值回收率均在90%~110%之间,RSD值均小于5%;6份BSA溶液的TOC值的SD为0.202 ppm,RSD为2.13%;碳浓度在0~20 ppm范围内的BSA溶液的加样TOC值与测得TOC值呈良好的线性关系,R2=0.999 5;检测用水的10次TOC检测值的LOD和LOQ值均明显低于10 ppm;两条回归曲线的决定系数的RSD为0.03%;不锈钢和玻璃材质擦拭取样的TOC检测值最低回收率分别为74%和77%,不同工作人员检测结果 RSD均≤20%。血液制品TOC检测擦拭法清洁验证结果均低于2μg/cm2。结论 TOC检测法具有良好的准确性、重复性、灵敏度、线性,血液制品清洁残留量均低于残留限度,达到预计的清洁效果。该方法快捷简便,适用于血液制品的擦拭法清洁验证。
Objective To establish a method for the validation of blood products cleaning with total organic carbon (TOC) analyzer. Methods A bovine serum albumin (BSA) solution with a carbon concentration of 5,10,15 ppm was prepared. The TOC value was measured and the recovery was calculated to verify the accuracy of the method. Six BSA samples with a carbon concentration of 10 ppm Solution, detecting the TOC value, calculating the relative standard deviation (RSD), and verifying the repeatability of the method; preparing BSA solutions with carbon concentrations of 0, 1, 2.5, 5, 10, 15 and 20 ppm, respectively, , And the linearity of the method was verified. The TOC value of 10 TOC water samples was determined, and the limit of detection (LOD) and limit of quantitation (LOQ) were calculated. The concentration of carbon was 0,1 , 2.5, 5, 10, 15 and 20 ppm of BSA solution. The concentrations of TOC were determined by analyzing the TOC values from low to high concentrations and from high to low concentrations. The regression coefficients were calculated and the residual effects were determined. Stainless steel and glass wipe samples, TOC detection, calculate the recovery and RSD. After cleaning the blood product manufacturing equipment and utensils wipe sampling, testing TOC value, confirm the cleaning effect. Results The TOC values of BSA solution at 3 carbon concentrations ranged from 90% to 110% and the RSD values were less than 5%. The TOC values of 6 BSA solutions were 0.202 ppm with RSD of 2.13% The TOC value of the BSA solution in the range of 0 ~ 20 ppm showed a good linear relationship with the measured TOC value, R2 = 0.999 5; the LOD and LOQ values of the 10 TOC values of the test water were significantly lower than 10 ppm; The RSD of the coefficient of determination of the two regression curves was 0.03%. The minimum recoveries of TOC values of stainless steel and glass wipe samples were 74% and 77%, respectively. The RSDs of different staffs were both ≤20%. Blood products TOC test wipe cleaning validation results were less than 2μg / cm2. Conclusion The TOC detection method has good accuracy, repeatability, sensitivity, linearity, and residues of blood products are lower than the residue limit, to achieve the expected cleaning effect. The method is quick and easy, suitable for wiping cleaning of blood products.