摘要
提出了气相色谱法(GC)和高效液相色谱法(HPLC)测定角膜塑形镜中甲基丙烯酸(MAA)、3-(异丁烯酰氧)丙基三(三甲基硅氧烷)硅烷(TRIS)、1,1,1,3,3,3-六氟异丙基异丁烯酸酯(HFIPM)等3种单体残留量的方法,并对两种方法的方法学验证与样品测定结果进行比较。取不少于200 mg的镜片样品,置于真空干燥箱中,于(60±5)℃真空条件下干燥不少于24 h至恒重。将恒重后的样品放入索氏提取器中,加入100 mL二氯甲烷,加热提取4~6 h。提取液转移至100 mL容量瓶中,用二氯甲烷定容,得到供试品溶液。GC采用DB-WAX毛细管色谱柱(30 m×0.32 mm,0.5μm),以氮气为载气,以柱升温程序方式分离,以氢火焰离子化检测器检测。HPLC采用CAPCELL PAK C_(18) MGⅡ色谱柱(150 mm×4.6 mm,5μm),以不同体积比的0.1%(体积分数)磷酸溶液和乙腈的混合溶液为流动相,以梯度洗脱方式分离,以二极管阵列检测器检测。结果显示:GC得到的标准曲线的线性范围为1.0~1 000 mg·L^(-1),检出限为0.006%~0.010%;HPLC得到的标准曲线的线性范围为0.1~200 mg·L^(-1)(MAA、HFIPM)和1.0~1 000 mg·L^(-1)(TRIS),检出限为0.001%~0.009%,表明GC适用于测定高残留量样品,HPLC适用于测定低残留量样品。GC所得回收率为89.1%~111%,测定值的相对标准偏差(RSD,n=6)为0.83%~4.1%;HPLC所得回收率为90.5%~108%,测定值的RSD(n=6)为0.92%~4.7%。在显著性水平为0.05条件下,经F检验和t检验分析,两种方法的测定结果无显著性差异。对3批来自不同生产企业的角膜塑形镜进行残留量和迁移量试验,结果显示:3批样品中均检出TRIS残留,TRIS的迁移量最大值为0.112%;2批样品中检出MAA残留,1批样品中检出HFIPM残留,而MAA和HFIPM均未在迁移量试验中检出。
Methods for the determination of residues of 3 monomers,including methacrylic acid(MAA),3-(methacryloyloxy) propyltris(trimethylsiloxy) silane(TRIS) and 1,1,3,3,3-hexafluoroisopropylisobutenolate(HFIPM) in orthokeratology lens by gas chromatography(GC) and high performance liquid chromatography(HPLC) were proposed,and the results of methodology validation and sample determination using the two methods were compared.The lens sample no less than 200 mg was placed into a vacuum drying oven and dried at(60±5)℃ under vacuum condition for no less than 24 h to constant weight.The sample with constant weight was put into a Soxhlet extractor,and 100 mL of dichloromethane was added for heating 4-6 h.The extraction solution was transferred into a 100 mL-volumetric bottle and diluted with dichloromethane to obtain the test solution.In the GC method,the separation was performed on DB-WAX capillary column(30 m×0.32 mm,0.5 μm) by column temperature program with nitrogen as carrier gas,and the targets were detected by flame ionization detector.In the HPLC method,the separation was carried out on CAPCELL PAK C_(18) MGⅡcolumn(150 mm×4.6 mm,5 μm) by gradient elution with the mixed solution composed of 0.1%(volume fraction) phosphoric acid solution and acetonitrile at different volume ratios as mobile phase,and the targets were detected by diode array detector.The results showed that the same linear range of the standard curves obtained by GC was 1.0-1 000 mg·L^(-1),with detection limits in the range of 0.006%-0.010%,and the linear ranges of the standard curves obtained by HPLC were 0.1-200 mg·L^(-1) for MAA and HFIPM,and 1.0-1 000 mg·L^(-1) for TRIS,with detection limits in the range of 0.001%-0.009%,indicating that GC was suitable for the determination of high residual samples and HPLC was suitable for the determination of low residual samples.The recoveries measured by GC were in the range of 89.1%-111%,with RSDs(n=6) of the determined values ranged from 0.83% to 4.1%,and the recoveries measured by HPLC were in the range of 90.5%-108%,with RSDs(n=6) of the determined values ranged from 0.92% to 4.7%.There was no significant difference between the two methods by F-test and t-test analysis at the significance level of 0.05.Three batches of orthokeratology lenses from different manufacturers were tested for residue and migration.The results showed that residual amount of TRIS was detected in three batches of samples,and the maximum migration amount of TRIS was 0.112%.Residual amount of MAA was detected in two batch of samples,and residual amount of HFIPM was detected in one batch of sample,but MAA and HFIPM were not detected in the migration test.
作者
徐萍华
鲍娇慧
张莉
诸丹
王安燕
XU Pinghua;BAO Jiaohui;ZHANG Li;ZHU Dan;WANG Anyan(Zhejiang Institute of Medical Device Supervision and Testing,Hangzhou 310018,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2023年第4期415-421,共7页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
