Establishment and optimization of inductively coupled plasma mass spectrometry (ICP-MS) for the determination of aluminum residues / 中国输血杂志

【Objective】 To establish and optimize a method for the determination of aluminum (Al) residue by inductively coupled plasma mass spectrometry (ICP-MS). 【Methods】 Nitric acid solution was used to treat samples and standards. The concentration of nitric acid solution and equipment parameters were optimized, and the specificity, linearity, repeatability, accuracy, detection limit, quantitative limit and intermediate precision of the optimized detection method were investigated to confirm whether it was suitable for the determination of Al residue in human serum albumin. 【Results】 The concentration of nitric acid was 5%, and digest time was 4 h. The equipment condition of ICP-MS was as follows: RF power: 1600 W, sampling depth: 10 mm, atomizer / carrier gas flow rate: 1.0 L/ min, compensation flow rate: 0.5 L/ min, experimental mode: standard mode, integration time: 0.2 s, data acquisition: 3 times. Specificity: The recoveries of Al: 92% (high concentration, RSD=3.5%), 98% (low concentration, RSD=4.9%). Linearity: In the range of (0~40) μg/L, the correlation coefficient between concentration and optical energy signal (CPS) of standard / sample were higher than 0.999 0. Accuracy/ Repeatability: The recoveries of sample (3 concentration): 108% (RSD=4.7%), 110% (RSD=4.9%) and 110% (RSD=2.8%). The detection limit was 0.006 μg/L, and the quantitation limit was 0.019 μg/L. Intermediate precision: personnel factor and date factor, P>0.05, RSD (12 times)=2%. Comparison between ICP-MS and atomic absorption spectrometry (AAS): the deviation between ICP-MS and AAS was 8%, and that of samples was 3%, with no significant difference noticed between the two methods. 【Conclusion】 After optimization, ICP-MS method has shown good performance in terms of specificity, linearity, repeatability, accuracy, detection limit, quantitative limit and intermediate precision, and is suitable for the determination of Al residue in human albumin products of our company.

The Analysis Methodology for Multiple Elements in Four Herbs ofSanjie Zhentong Capsules / 世界科学技术-中医药现代化

To develop a method for the determination of 18 elements such as Pb, Cu, As, Hg, Mn, Ni, & Tl in Panax notoginseng,Bulbus fritillariae thunbergii,Coix seed, Resina draconis, and to control the contents of heavy metal elements in Sanjie Zhentong Capsule, the samples were digested by microwaves and then analyzed by appropriate determination parameters through ICP-MS, with the internal standard method to improve the matrix effect and interference. The correlation coefficientR2≥ 0.999 2. The lowest limits of quantification were from 0.002 8 to 0.54 μg·L-1. The experiments had better repeatability, while the recovery values ranged from 73.01% to 109.13%. The method is simple, accurate and high sensitive, and it can be used for the determination of rapid monitoring the multi-elements inPanax notoginseng, Bulbus fritillariae thunbergii, Coix seed,and Resina draconis.