机构地区:[1]泰安市食品药品检验检测研究院(泰安市纤维检验所)药品科,271000
出 处:《中国实用医药》2025年第3期177-180,共4页China Practical Medicine
摘 要:目的探讨蒸馏法和碱性超声波浸提法快速检测中药饮片中二氧化硫(SO_(2))残留量的效果。方法以茯苓、菊花、山药、白术、甘草等16种中药饮片样本为研究对象,其中白色样本以碱性超声波浸提法测定SO_(2)含量,有色样本以蒸馏法测定SO_(2)含量,观察测定结果并以国标酸碱滴定法(ABT)测定SO_(2)结果为对照,评价两种方法的检测效果。结果SO_(2)值在1.0~13.5μg内线性关系良好(r=0.98)。根据计算公式,碱性超声波浸提法SO_(2)检测限为0.20μg,蒸馏法SO_(2)检测限为0.22μg,两种方法最低检测浓度均为10 mg/kg。根据试验结果,6份茯苓供试品溶液SO_(2)的残留量分别为244.2、239.8、241.7、242.5、244.6、240.9 mg/kg,经计算RSD为1.27%。6份菊花供试品溶液SO_(2)的残留量分别为81.7、82.8、80.9、81.4、83.6、82.2 mg/kg,经计算RSD为1.03%,重复性均较好。根据计算,碱性超声波浸提法(茯苓样本)与蒸馏法(菊花样本)的回收率均在90%以上。通过对比,蒸馏法与碱性超声波浸提法对12种中药饮片样本中SO_(2)残留量的测定结果与国标ABT差别不大,SO_(2)相差比多数在5%以内,最大为百合(7.30%),未超过8%。结论蒸馏法与碱性超声波浸提法操作简单,测定中药饮片SO_(2)残留量的结果与国标ABT差别不大,适宜在药品检测与监管部门中推广应用。Objective To explore the effect of rapid determination of sulfur dioxide(SO_(2))residue in Chinese herbal slices by distillation method and alkaline ultrasonic extraction method.Methods The samples of 16 kinds of Chinese herbal slices,including Poria cocos,chrysanthemum,yam,atractylodes macrocephala,and licorice,were taken as the research objects.The content of SO_(2)in white samples was determined by alkaline ultrasonic extraction method,and the content of SO_(2)in colored samples was determined by distillation method.The results were observed and compared with the results of SO_(2)determination by national standard acid-base titration(ABT)to evaluate the detection effect of the two methods.Results SO_(2)values showed good linearity(r=0.98)within 1.0-13.5μg.The detection limits of distillation method and alkaline ultrasonic extraction method were 0.22 and 0.20μg,and the minimum detection concentration was 10 mg/kg for both methods.According to the test results,the residues of SO_(2)in the 6 samples of Poria Cocos were 244.2,239.8,241.7,242.5,244.6,240.9 mg/kg,respectively,and the calculated RSD was 1.27%;the residues of SO_(2)in 6 samples of chrysanthemum were 81.7,82.8,80.9,81.4,83.6,82.2 mg/kg,and the calculated RSD was 1.03%,with good repeatability.According to the calculation,the recoveries of alkaline ultrasonic extraction method(Poria cocos sample)and distillation method(chrysanthemum sample)were both above 90%.By comparison,the difference between the SO_(2)residue of 12 kinds of Chinese medicine decoction pieces measured by distillation and alkaline ultrasonic extraction method and the SO_(2)test results of national standard ABT was less than 5%in most cases,with the largest difference being for lilies(7.3%),not exceeding 8%.Conclusion The method of distillation and alkaline ultrasonic extraction is simple,and the results of SO_(2)determination are not different from the national standard ABT,which is suitable for promotion in drug testing and supervision departments.
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