邻苯二甲酸酯类标准物质核磁共振定量方法的建立

目的 :建立以核磁共振定量法(简称qNMR法)测定邻苯二甲酸酯标准物质含量. 方法 :仪器为配备5 mm BBO探头的Bruker Ascend 500 MHz核磁共振仪,采集一维定量氢谱,90°脉冲,延迟时间的d1为20 s,温度为25 ℃,采样次数为128次.以富马酸为内标,对12种邻苯二甲酸酯类标准物质进行定量研究. 结果 :12种邻苯二甲酸酯标准物质qNMR法测定结果与对照品标定的质量平衡法定值结果基本一致. 结论: 采用qNMR法研究建立邻苯二甲酸酯标准物质含量测定方法,方法快捷、准确,是对标准物质量值定量测定的一种良好的补充.

Objective: To develop a nuclear magnetic resonance(qNMR) method for the quantitative determination of phthalate esters standard materials. Methods: ¹H-NMR spectra were collected at Bruker Ascend 500 spectrometer with 5 mm BBO probe.The internal standard was fumaric acid.The parameter setup was as follows: 90° pulse sequences,d1 was 20 s,temperature was 25 ℃,and the number of scan was 128. Results: The qNMR results of 12 phthalate esters standard materials were consistent with the results obtained from mass balance methods. Conclusion: qNMR method is a good supplementary quantitative method for standard materials,which can be used for the rapid quantitative determination of phthalate esters standard materials.

[1] ALBERT O,JEGOU B.A critical assessment of the endocrine susceptibility of the human testis to phthalates from fetal life to adulthood[J].Human Reprod Update,2014,20(2):231
[2] KIM SH,PARK MJ.Phthalate exposure and childhood obesity[J].Annal Pediatric Endocrinol Metabol,2014,19(2):69
[3] BAJKIN I,BJELICA A,ICIN T,et al.Effects of phthalic acid esters on fetal health[J].Med Preg,2014,67(5/6):172
[4] LOTTRUP G,ANDERSSON AM,LEFFERS H,et al.Possible impact of phthalates on infant reproductive health[J].Int J Androl,2006,29(1):172; discussion 181
[5] HEUDORF U,MERSCH-SUNDERMANN V,ANGERER J.Phthalates: toxicology and exposure[J].Int J Hyg Environ Health,2007,210(5):623
[6] ZHOU J,QI Y,WU H,et al.Simultaneous determination of trace migration of phthalate esters in honey and royal jelly by GC-MS[J].J Sep Sci,2014,37(6):650
[7] LIU Y,WANG S,WANG L.Development of rapid determination of 18 phthalate esters in edible vegetable oils by gas chromatography tandem mass spectrometry[J].J Agric Food Chem,2013,61(6):1160
[8] XU D,DENG X,FANG E,et al.Determination of 23 phthalic acid esters in food by liquid chromatography tandem mass spectrometry[J].J Chromatogr A,2014,1324():49
[9] GK H,HUANG T,YANG Y,et al.Purity determination and uncertainty evaluation of folic acid by mass balance method[J].Talanta,2012,101():96
[10] MAHAJAN S,SINGH IP.Determining and reporting purity of organic molecules: why qNMR[J].Magn Reson Chem,2013,51(2):76
[11] JUNGNICKEL JL,FORBES JW.Quantitative measurement of hydrogen types by intergrated nuclear magnetic resonance intensities[J].Anal Chem,1963,35(8):938
[12] MANIARA G,RAJAMOORTHI K,RAJAN S,et al.Method performance and validation for quantitative analysis by (1)H and (31)P NMR spectroscopy.Applications to analytical standards and agricultural chemicals[J].Anal Chem,1998,70(23):4921
[13] ZHANGQ(张琪),LI XD(李晓东),YANG HX(杨化新).Application of nuclear magnetic resonance in pharmaceutical standards(核磁共振技术在药品标准领域中的应用进展)[J].Chin J Pharm Anal(药物分析杂志),2012,32(3):545
[14] WEI YL(韦英亮),MO JG(莫建光),PAN YK(潘艳坤).A quantitative NMR method for period verification of sulfonamides reference materials(磺胺类标准物质期间核查NMR定量方法研究)[J].Chin J Mag Reson(波谱学杂志),2013,30(3):371
[15] HU M(胡敏),HU CQ(胡昌勤),LIU WY(刘文英).Determination of drug reference substance content by 1 H-nuclear magnetic resonance (NMR) spectroscopy(核磁共振波谱法测定药物基准物质的绝对含量)[J].Chin J Anal Chem(分析化学杂志),2004,32(4):451
[16] ZHANG YJ(张友杰),LIU XP(刘小鹏).Studies of NMR acquisition parameters for quantitative analysis of drugs(药物核磁共振定量分析参数的研究)[J].Chin J Mag Reson(波谱学杂志),2007,24(3):289.
[17] ZHANGQ(张琪),YANGHX(杨化新),XIAOXY(肖新月),et al.Quantitative nuclear magnetic resonance determination of ambroxol hydrochloride impurities(核磁共振法定量测定盐酸氨溴索杂质)[J].Chin J Pharm Anal(药物分析杂志),2014,34(11):2030
[18] RUNDLOF T,MATHIASSON M,BEKIROGLU S,et al.Survey and qualification of internal standards for quantification by 1H NMR spectroscopy[J].J Pharm Biomed Anal,2010,52(5):645
[19] PAULI GF,JAKI BU,LANKIN DC.Quantitative ¹H NMR: development and potential of a method for natural products analysis[J].J Nat Prod,2005,68(1):133