SN∕T 5324.1-2020 出口包装饮用水和饮用天然矿泉水中奥卡西平、阿米替林、舍曲林、帕罗西汀和阿利马嗪的测定 液相色谱-质谱质谱法(出入境检验检疫).pdf

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1、以正式出版文本为准中华人民共和国出入境检验检疫行业标准SN/T 5324.12020出口包装饮用水和饮用天然矿泉水中奥 卡西平、阿米替林、舍曲林、帕罗西汀 和阿利马嗪的测定 液相色谱-质谱/质谱法Determination of oxcarbazepine,amitriptyline,sertraline,paroxetine and alimemazine in exported packaged drinking water and drinking natural mineral water-LC-MS/MS method2020-12-30 发布2021-07-01 实施ICS 67.

2、160CCS X 51中华人民共和国海关总署发 布以正式出版文本为准以正式出版文本为准SN/T 5324.12020I前 言本文件按照 GB/T 1.1 2020给出的规则起草。请注意本文件的某些内容可能涉及专利。本文件的发布机构不承担识别这些专利的责任。本文件由中华人民共和国海关总署提出并归口。本文件起草单位：中华人民共和国北京海关、北京市食品科学研究院。本文件主要起草人：梁娜娜、冯鑫、韩深、王珮玥、古瑾、刘萤、崔凤云、齐鹤鸣。以正式出版文本为准以正式出版文本为准1SN/T 5324.12020出口包装饮用水和饮用天然矿泉水中奥 卡西平、阿米替林、舍曲林、帕罗西汀 和阿利马嗪的测定 液相色谱

3、-质谱/质谱法1 范围本文件规定了饮用纯净水、饮用天然矿泉水和其他饮用水中奥卡西平、阿米替林、舍曲林、帕罗西汀和阿利马嗪的液相色谱-质谱/质谱检验方法。本文件适用于饮用纯净水、饮用天然矿泉水和其他饮用水中奥卡西平、阿米替林、舍曲林、帕罗西汀和阿利马嗪的测定。2 规范性引用文件下列文件中的内容通过文中的规范性引用而构成本文件必不可少的条款。其中，注日期的引用文件，仅该日期对应的版本适用于本文件；不注日期的引用文件，其最新版本（包括所有的修改单）适用于本文件。GB/T 33087 仪器分析用高纯水规格及试验方法3 术语和定义本文件没有需要界定的术语和定义。4 方法提要试样中的待测物经液相色谱-质谱

4、/质谱进行分离和测定，外标法定量。5 试剂和材料除另有说明外，所用试剂均为色谱纯，水为符合 GB/T 33087 规定的仪器分析用高纯水。5.1 甲酸。5.2 甲醇。5.3 乙腈。5.4 0.5%甲酸：5 mL 甲酸溶解于水中，并定容至 1 L。5.5 20%甲醇：20 mL 甲醇溶解于水中，并定容至 100 mL。5.6 奥卡西平标准物质：C15H12N2O2，CAS 28721-07-5，纯度99%。5.7 阿米替林标准物质：C20H23N，CAS 50-48-6，纯度99%。5.8 舍曲林标准物质：C17H17Cl2N，CAS 79617-96-2，纯度99%。以正式出版文本为准2SN/

5、T 5324.120205.9 帕罗西汀标准物质：C19H20FNO3，CAS 61869-08-7，纯度99%。5.10 阿利马嗪标准物质：C18H22N2S，CAS 84-96-8，纯度99%。5.11 标准储备液：分别准确称取标准物质奥卡西平（5.6）、阿米替林（5.7）、舍曲林（5.8）、帕罗西汀（5.9）和阿利马嗪（5.10）各 10 mg（精确至 0.1 mg）于 10 mL 棕色容量瓶中，分别用甲醇（5.2）溶解并定容至刻度，配制成浓度为 1 000 mg/L 的标准储备溶液，于-18 避光保存。5.12 混合标准中间溶液：分别取标准储备液（5.11）0.1 mL 混合，用甲醇（

6、5.2）定容于 10 mL 容量瓶，制成浓度 10 mg/L 的混合标准中间溶液，于 4 避光保存。5.13 混合标准工作溶液：用 20%甲醇（5.5）稀释成 0.1 ng/mL、0.5 ng/mL、5 ng/mL、20 ng/mL、40 ng/mL 等系列浓度的混合标准工作溶液，使用前配制。6 仪器和设备6.1 高效液相色谱-质谱/质谱仪：配有电喷雾离子源（ESI）。6.2 天平：感量为 0.1 mg。6.3 高速离心机：转速10 000 r/min。6.4 具塞塑料离心管：2 mL。6.5 尼龙微孔滤膜：0.22 m。7 测定步骤7.1 试样的制备将水样摇匀静置10 min后，取适量水样置

7、于具塞塑料离心管（6.4），于12 000 r/min 离心5 min后，上清液过 0.22 m 微孔滤膜（6.5）后待上机。7.2 试样的保存将试样于 4 避光保存。7.3 测定7.3.1 液相色谱条件液相色谱条件如下：a）色谱柱：HSS T3，100 mm 2.1 mm，粒径 1.7 m，或相当者；b）进样体积：5 L；c）柱温：40 ；d）流速：0.35 mL/min；e）液相色谱流动相及参考分离条件见表 1。表 1 液相色谱梯度洗脱程序时间/min乙腈/%0.5%甲酸水溶液/%0.05.0 95.0 0.55.0 95.0 3.030.0 70.0 以正式出版文本为准3SN/T 532

8、4.12020表 1（续）时间/min乙腈/%0.5%甲酸水溶液/%9.095.0 5.0 10.095.0 5.0 10.55.0 95.0 12.05.0 95.0 7.3.2 质谱条件质谱条件如下：a）离子化模式：电喷雾离子源（ESI+）；b）扫描方式：多反应监测模式（MRM）；c）使用前应调节各参数使质谱灵敏度达到检测要求，参考条件参见附录 A。7.3.3 定性测定按照液相色谱-质谱/质谱条件测定样品和标准工作溶液，如果检测的质量色谱峰保留时间与标准品保留时间相差不超过 5%，定性离子对相对丰度（是用相对于最强离子丰度的强度百分比表示）与浓度相当的标准工作溶液的相对丰度一致，相对丰度允

9、许偏差不超过表 2 规定的范围，则可判定样品中存在对应的待测物。表 2 定性确证时相对离子丰度的最大允许偏差相对离子丰度/%5020501020 10允许的相对偏差/%202530507.3.4 定量测定根据试样中被测物的含量情况，选取响应值相近的标准工作液一起进行色谱分析。标准工作液和待测中奥卡西平、阿米替林、舍曲林、帕罗西汀和阿利马嗪的响应值应在仪器线性范围内。样品溶液中的参考保留时间参见附录 A。样液中奥卡西平、阿米替林、舍曲林、帕罗西汀和阿利马嗪多反应监测（MRM）色谱图参见附录 B。7.3.5 空白试验用水代替样品，按上述步骤进行。8 结果计算和表述样品中奥卡西平、阿米替林、舍曲林、

10、帕罗西汀和阿利马嗪的测定结果按照式（1）计算用色谱数据处理器或按式（1）计算试样中待测物的残留量，计算结果需扣除空白：Xi=cif（1）式中：Xi试样中待测物的残留量，单位为纳克每毫升（ng/mL）；以正式出版文本为准4SN/T 5324.12020ci 由标准工作曲线得到的样液中某待测物的浓度，单位为纳克每毫升（ng/mL）；f 样品的稀释倍数。计算结果保留三位有效数字。9 定量限和回收率9.1 定量限本方法中奥卡西平、阿米替林、舍曲林、帕罗西汀和阿利马嗪的定量限均为 0.1 ng/mL。9.2 回收率在饮用纯净水、饮用天然矿泉水、其他饮用水基质中添加奥卡西平、阿米替林、舍曲林、帕罗西汀和阿

11、利马嗪，添加水平及回收率的实验数据见表 3。表 3 奥卡西平、阿米替林、舍曲林、帕罗西汀和阿利马嗪的添加回收率试验数据（n=6）化合物添加水平 ng/mL回收率范围（%）饮用纯净水其他饮用水饮用天然矿泉水奥卡西平0.187.0-106.090.0-111.089.0-112.00.291.0-111.587.5-108.086.5-111.5190.6-113.585.9-112.097.9-111.7阿米替林0.187.0-111.085.0-107.092.0-112.00.294.5-114.585.5-109.088.0-114.0190.5-102.388.3-113.586.0-9

12、7.0舍曲林0.185.0-110.086.0-112.089.0-114.00.288.0-112.585.5-110.092.5-112.0187.9-110.688.8-110.386.7-111.9帕罗西汀0.191.0-113.092.0-112.088.0-113.00.290.0-107.591.0-113.088.0-114.5186.1-106.189.4-113.398.8-109.2阿利马嗪0.188.0-114.086.0-108.091.0-111.00.289.0-109.588.0-111.086.0-114.0189.4-113.790.6-108.095.3-

13、114.4以正式出版文本为准5SN/T 5324.12020附 录 A（资料性）质谱参数1）A.1 液相色谱-质谱/质谱参数如下：a）毛细管电压：1.00 kV；b）去溶剂气温度：500 ；c）去溶剂气流速：1 000 L/Hr；d）碰撞气流速：0.14 mL/min；e）离子源温度：150 ；f）雾化气压力：6.0 bar。g）定性定量离子等其他参数见表 A.1。表 A.1 主要质谱参数化合物保留时间/min母离子 m/z子离子 m/z锥孔电压（V）碰撞电压（eV）奥卡西平4.67253.1 180.0*2028253.1 166.92034阿米替林6.51278.291.0*3522278

14、.2105.0 3524舍曲林6.85306.1158.9*2028306.1275.0 2010帕罗西汀5.99330.270.1*3528330.2192.1 3520阿利马嗪6.36299.1100.1*2018299.1212.0 2024注:带*的离子为定量离子。1）非商业性声明：附录 A 所列参数是在 Waters Xevo TQ-S 质谱仪上完成的，此处列出试验用仪器型号仅是为了提供参考，并不涉及商业目的，鼓励标准使用者尝试采用不同厂家或型号的仪器。以正式出版文本为准6SN/T 5324.12020附 录 B（资料性）多反应监测（MRM）色谱图图 B.1 多反应监测（MRM）色谱

15、图习奥卡西平4.67 253.096 180.026 1.38e7 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 4.67 253.096 166.959 1.72e6 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 3阿束?林6.51 278.16 105.046 1.02e7 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 6.51 278.16 91.066 1.40e7 1.00 2.00 3.00 4.00 5.00 6.

16、00 7.00 8.00 9.00 10.00 10挨11斗告曲林6.85 306.096 274.975 1.74e6 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 6.85 306.096 158.869 2.62e6 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 3帕罗西汀5.99 330.16 192.093 5.67e6 0,1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 5.99 330.16 70.067 6.78e

17、6 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 可阿利马嚓6.36 299.096 211.984 3.6ge6 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 6.36 299.096 100.085 3.64e7 Time 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 以正式出版文本为准7SN/T 5324.12020ForewordThis standard is drafted according to GB/T 1.1

18、2020,GB/T 20001.42015 and SN/T 00012016.Please note that some of the contents of this document may involve patents.The issuing body of this document does not undertake the responsibility of identifying these patents.This standard is proposed by and is under the jurisdiction of General Administration

19、 of Customs,P.R.China.The standard is drafted by Beijing Customs District P.R.China,Beijing Academy of Food Science.The main drafters of this standard are Liang Nana,Feng Xin,Han Shen,Wang Peiyue,Gu Jin,Liu Ying,Cui Fengyun and Qi Heming.以正式出版文本为准8SN/T 5324.12020Determination of oxcarbazepine,amitri

20、ptyline,sertraline,paroxetine and alimemazine in exported packing drinking water and drinking natural mineral water-HPLC-MS/MS method1 ScopeThis standard specifies the determination method of oxcarbazepine,amitriptyline,sertraline,paroxetine and alimemazine,in purified drinking water,natural drinkin

21、g mineral water and other drinking water by HPLC-MS/MS method.This standard is applicable to the determination of oxcarbazepine,amitriptyline,sertraline,paroxetine and alimemazine in purified drinking water,natural drinking mineral water and other drinking water.2 Normative referenceThe following do

22、cument is necessary for this standard.For dated reference,only dated editions shall apply to this standard.For undated references,the latest edition of the normative document referred to apply.GB/T 33087 Ultra pure water for instrumental analysis specification and test methods3 Terms and definitions

23、There are no terms and definitions to be defined in this document.4 PrincipleThe compounds in samples are separated and determinated directly by HPLC-MS/MS.External standard method is used to determine the concentration of compounds.5 Regents and materialsUnless otherwise specified,all the regents u

24、sed should be chromatographic grade.“Water”is the ultra pure water for instrumental analysis prescribed by GB/T 33087.5.1 Formic acid.5.2 Methanol.5.3 Acetonitrile.5.4 0.5%Formic acid water solution:5 mL formic acid is dissolved in water and is fixed to 1 L.5.5 20%Methanol water solution:20 mL metha

25、nol is dissolved in water and is fixed to 100 mL.5.6 Oxcarbazepine standards:C15H12N2O2，CAS 28721-07-5，purity:99%.5.7 Amitriptyline standards:C20H23N,CAS 50-48-6,purity:99%.5.8 Sertraline standards:C17H17Cl2N,CAS 79617-96-2,purity:99%.以正式出版文本为准9SN/T 5324.120205.9 Paroxetine standards:C19H20FNO3,CAS

26、61869-08-7,purity:99%.5.10 Alimemazine standards:C18H22N2S,CAS 84-96-8,purity:99%.5.11 Standard stock solution:separately weigh 10 mg of oxcarbazepine（5.6）,amitriptyline（5.7）,sertraline（5.8）,paroxetine（5.9）and alimemazine（5.10）（to the nearest 0.1 mg）and dissolve in a small amount of methanol,then fi

27、ll to the volume of 10 mL using methanol.The concentration of each standard stock solution is 1 000 mg/L and stored at-18 .5.12 Standard mix intermediate concentration solution:accurately pipette 0.1 mL of each standard stock solution（5.11）.Fill to the volume of 10 mL using methanol.The concentratio

28、n of each standard is 10 mg/L in the mix intermediate concentration solution and stored at 4 .5.13 Standard mix working solution:Pipette adequate amount of standard mix intermediate concentration solution（5.11）,dilute with 20%Methanol water solution（5.5）to prepare appropriate concentration standard

29、working solutions before use.For oxcarbazepine,amitriptyline,sertraline,paroxetine and alimemazine,the concentration of these working solutions are 0.1,0.5,5,20,40 ng/mL.6 Apparatus and equipment6.1 High performance liquid chromatography:equipped with electric spray ion source（ESI）.6.2 Analytical ba

30、lance:a sensitivity of 0.1 mg.6.3 Centrifuge:10 000 r/min.6.4 Plugged plastic centrifuge tube:2 mL.6.5 Millipore filter film:0.22 m,nylon.7 Procedure7.1 Sample preparationStand the water samples for 10 min after shaking it.Pipet a small amount of sample to the 2 mL plug plastic centrifuge tube（6.4）a

31、nd centrifuge for 5 min at 12 000 r/min.Filter the supernatant with millipore filter film（6.5）for LC-MS/MS analysis.7.2 Sample storageThe test samples should be stored at 4 .7.3 Determination7.3.1 HPLC operation conditionsHPLC operation conditions are as follows:a）Chromatographic column:HSS T3,100 m

32、m2.1 mm（inner diameter）,1.7 m or equivalent；b）Injection volume:5 L；c）Column temperature:40 ；d）Flow rate:0.35 mL/min；e）Liquid phase and separation conditions:according to table 1.以正式出版文本为准10SN/T 5324.12020Table 1 Liquid chromatography gradient elution procedureTime/minAcetonitrile/%0.5%Formic acid/%0

33、.05.0 95.0 0.55.0 95.0 3.030.0 70.0 9.095.0 5.0 10.095.0 5.0 10.55.0 95.0 12.05.0 95.0 7.3.2 Mass spectrometry operation conditionsMass spectrometry operation conditions are as follows:a）Ion source:electric spray ion source（ESI+）；b）Scan mode:multiple reaction monitoring model（MRM）；c）The parameters s

34、hould be adjusted before use to make the sensitivity of the mass spectrum meet the testing requirements.Refer to appendix A for reference conditions.7.3.3 Qualitative determinationThe sample and standard working solution are determined according to the liquid chromatography mass spectrometry/mass sp

35、ectrometry conditions.The variation range of the retention time for the peaks in unknown sample and in the standard solution cannot be out of the range of 5%.For the same analysis batch and same compound,the variation range of the ion ratio of the two product ions for the unknown sample and the work

36、ing standard solution at the similar concentration can not be out of the range of table 2.Table 2 Maximum permitted tolerance for relative ion intensities while conformationRelative intensity/%5020501020 10Permitted tolerance/%202530507.3.4 Quantification determinationAccording to the content of the

37、 tested substance in the sample,the standard working solution with similar response value is selected for chromatographic analysis.Under the optimum working conditions,the standard working solution is detected with similar response to that of sample solution.The response of oxcarbazepine,amitriptyli

38、ne,sertraline,paroxetine and alimemazine in the standard working solution and sample solution should be in the linear range of the instrumental detection,using external calibration curve for quantitative analysis.The retention time and the multiple reaction monitoring model（MRM）chromatograms of oxca

39、rbazepine,amitriptyline,sertraline,paroxetine and alimemazine are shown in annex A and annex B,separately.7.3.5 Blank testThe operation of blank test is the same as the described in the method of determination,but with samples 以正式出版文本为准11SN/T 5324.12020replaced by ultra pure wate for instrumental an

40、alysis.8 Calculation and expression of the result Oxcarbazepine,Amitriptyline,Sertraline,Paroxetine and Alimemazine in the test sample are calculated using formula（1）.Calculate the content of analytes in the test sample using LC-MS data processor and the formula（1）.The blank value should be subtract

41、ed from the result of calculation:Xi=cif（1）Where:Xithe residue content of analytes,ng/mL；ci the concentration of analytes in the testing sample solution gained by standard curve,ng/mL；f the sample dilution ratio.The results are rounded off to three significant figures.9 Limit of quantification and r

42、ecovery9.1 Limit of quantificationThe limit of quantification for oxcarbazepine,amitriptyline,sertraline,paroxetine and alimemazine in purified drinking water,natural drinking mineral water and other drinking water are 0.1 ng/mL.9.2 RecoveryThe recovery data in different spiked levels of oxcarbazepi

43、ne,amitriptyline,sertraline,paroxetine and alimemazine in purified drinking water,natural drinking mineral water and other drinking water are listed in table 3.Table 3 The spiked levels and recovery ranges of oxcarbazepine,amitriptyline,sertraline,paroxetine and alimemazine in purified drinking wate

44、r,natural drinking mineral water and other drinking water（n=6）CompoundSpiked level/（ng/mL）Recovery range（%）Purified drinking waterOther drinking waterNatural drinking mineral waterOxcarbazepine0.187.0-106.090.0-111.089.0-112.00.291.0-111.587.5-108.086.5-111.5190.6-113.585.9-112.097.9-111.7Amitriptyl

45、ine0.187.0-111.085.0-107.092.0-112.00.294.5-114.585.5-109.088.0-114.0190.5-102.388.3-113.586.0-97.0Sertraline0.185.0-110.086.0-112.089.0-114.00.288.0-112.585.5-110.092.5-112.0187.9-110.688.8-110.386.7-111.9以正式出版文本为准12SN/T 5324.12020Table 3（续）CompoundSpiked level/（ng/mL）Recovery range（%）Purified drin

46、king waterOther drinking waterNatural drinking mineral waterParoxetine0.191.0-113.092.0-112.088.0-113.00.290.0-107.591.0-113.088.0-114.5186.1-106.189.4-113.398.8-109.2Alimemazine0.188.0-114.086.0-108.091.0-111.00.289.0-109.588.0-111.086.0-114.0189.4-113.790.6-108.095.3-114.4以正式出版文本为准13SN/T 5324.1202

47、0Annex A（Informative）The liquid chromatography-mass spectrometry/mass spectrometry parameters1）A.1 The liquid chromatography-mass spectrometry/mass spectrometry parameters are as follows:a）Capillary Voltages:1.00 kV；b）Desolvation Temperature:500 ；c）Desolvation Gas Flow:1 000 L/Hr；d）Collision Gas Flo

48、w：0.14 mL/min；e）Source Temperature:150 ；f）Nebuliser Pressure:6.0 bar；g）Qualitative and quantitative ions and optimized cone voltage and collision energy can be referred in Annex A.1.Table A.1 The liquid chromatography-mass spectrometry/mass spectrometry parametersCompoundRetention time（min）Precursor

49、 ion（m/z）Product ion（m/z）Cone voltage（V）Collision energy（eV）Oxcarbazepine4.67253.1 180.0*2028253.1 166.92034Amitriptyline6.51278.291.0*3522278.2105.0 3524Sertraline6.85306.1158.9*2028306.1275.0 2010Paroxetine 5.99330.270.1*3528330.2192.1 3520Alimemazine6.36299.1100.1*2018299.1212.0 2024Annotation:Th

50、e symbol“*”represents the quantitative ion.1）Non-commercial statement:The reference mass parameters in Annex A are accomplished by Waters Xevo TQ-S.The equipment and its type involved in the standard method is only for reference and not related to any commercial aim,and the analysts are encouraged t