摘要
采用题示方法测定具有代表性的市售亲水性丙烯酸酯类人工晶状体产品中5种小分子物质甲基丙烯酸羟乙酯(HEMA)、甲基丙烯酸乙氧基乙酯(EOEMA)、二甲基丙烯酸乙二醇酯(EGDMA)、三羟甲基丙烷三甲基丙烯酸酯(TMPTMA)、2-[3-(2H-苯并三唑-2-基)-4-羟苯基]甲基丙烯酸乙酯(UVE)的含量。将人工晶状体样品于(60±2)℃干燥至恒重,分取约0.2 g,加入浸提溶剂正己烷160 mL,于70℃索氏浸提,浸提速率为5次·h^(-1),共浸提5 h。取全部浸提液,蒸发至近干,用正己烷定容至10 mL,所得完全浸提液采用气相色谱-质谱法分析。取上述样品的原料晶胚约1.1 g,加入11 mL正己烷,于(35±2)℃(模拟人眼部温度)静置72 h,取出原料晶胚,所得溶出浸提液采用气相色谱-质谱法分析。在色谱分析中,以SH-Rxi-5MS色谱柱为固定相,在初始柱温80℃、柱升温速率10℃·min^(-1)和15℃·min^(-1)、进样口温度250℃、进样量1μL条件下高压进样;在质谱分析中,以电子轰击离子(EI)源电离,选择离子监测模式检测,外标法定量。结果显示:5种小分子物质的质量浓度均在一定范围内与峰面积呈线性关系,检出限(3S/N)为0.001~0.008 mg·L^(-1);按照标准加入法进行回收试验,回收率为90.3%~111%,测定值的相对标准偏差(n=6)小于5.0%。方法用于实际样品的分析,完全浸提液中除UVE外其他4种小分子物质的含量均小于溶出浸提液中的;溶出浸提液中UVE的含量明显高于其他4种小分子物质的,推测UVE为物理掺杂入原料晶胚。
The 5 small molecule substances,including hydroxyethyl methacrylate(HEMA),ethoxyethyl methacrylate(EOEMA),ethylene glycol dimethacrylate(EGDMA),trimethylolpropane trimethacrylate(TMPTMA),and 3-(2H-benzo[d][1,2,3]triazol-2-yl)-4-hydroxyphenethyl methacrylate(UVE),in essential commercially available hydrophilic acrylic intraocular lens products were determined by the method mentioned by the title.The intraocular lens sample was dried at(60±2)℃to a constant mass,about 0.2 g of which was taken.The 160 mL of extraction solvent(n-hexane)was added,and Celsius Soxhlet extraction was made at 70℃,repeatedly extracting 5 times within 1 h for a total of 5 h.All the extraction solution was collected,and evaporated to near dryness,and the resulting solution was made its volume up to 10 mL with n-hexane.The complete extraction solution obtained was analyzed by gas chromatography-mass spectrometry.About 1.1 g of the raw material embryo of the above sample was taken,and 11 mL of n-hexane was added.The mixture was settled at(35±2)℃(simulating human eye temperature)for 72 h,and then the raw material embryo was taken.The dissolution extract obtained was analyzed by gas chromatography-mass spectrometry.In chromatographic analysis,a SH-Rxi-5MS column was used as the stationary phase,and high-pressure injection was carried out under the conditions of initial column temperature of 80℃,column heating rate of 10℃·min^(-1) and 15℃·min^(-1),injection port temperature of 250℃,and injection volume of 1μL.In mass spectrometry analysis,EI source was used for ionization,selected ion monitoring mode was used for detection,and external standard method was used for quantification.It was shown that linear relationships between values of the mass concentrations and peak areas of the 5 small molecule substances were kept in definite ranges,with detection limits(3S/N)in the range of 0.001-0.008 mg·L^(-1).Test for recovery was made by the standard addition method,giving recoveries in the range of 90.3%-111%,and RSDs(n=6)of the determ
作者
徐柏杨
郭采妮
刘子琪
付步芳
付海洋
XU Baiyang;GUO Caini;LIU Ziqi;FU Bufang;FU Haiyang(National Institutes for Food and Drug Control,Beijing 102629,China;School of Materials Science and Engineering,Beihang University,Beijing 100191,China;School of Pharmacy,China Pharmaceutical University,Nanjing 211198,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2024年第12期1269-1274,共6页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
华南生物医用材料与植入器械创新示范基地项目(2017YFC1105000)。
关键词
气相色谱-质谱法
人工晶状体
小分子物质
正己烷
浸提
gas chromatography-mass spectrometry
intraocular len
small molecule substance
n-hexane
extraction
