水質硝基呋喃、大環(huán)內酯、氯霉素類、硝基咪唑類和抗病毒類藥物的測定

（資料性附錄）方法檢出限和測定下限表A.1給出了17種目標物的方法檢出限和測定下限。表A.1方法檢出限和測定下限序號目標化合物英文名稱CASNo.地表水、地下水和海水廢水方法檢出限（ng/L）測定下限（ng/L）方法檢出限（ng/L）測定下限（ng/L）1呋喃唑酮Furazolidone67-45-8284162呋喃它酮Furaltadone139-91-3284163呋喃西林Nitrofurazone59-87-0284164呋喃妥因Nitrofurantoin67-20-9284165紅霉素Erythromycin114-07-8284166泰樂菌素Tylosin1401-69-0284167白霉素Kitasamycin1392-21-8284168延胡索酸泰妙菌素Tiamulinfumarate55297-96-6284169林可霉素Lincomycin154-21-22831210替米考星Tilmicosin108050-54-02831211氯霉素Chloramphenicol56-75-70.62.42812甲砜霉素Thiamphenicol15318-45-30.72.82813氟甲砜霉素Florfenicol73231-34-20.72.82814甲硝唑Metronidazole443-48-10.62.42815二甲硝咪唑Dimetridazole551-92-80.72.82816洛硝達唑Ronidazole7681-76-70.72.82817金剛烷胺Amantadine768-94-50.62.428（資料性附錄）目標化合物及內標物的測定參考參數表B.1給出了目標化合物及內標物的保留時間、定量內標、多離子反應監(jiān)測條件等測定參考參數。表B.1目標化合物及內標物的保留時間、定量內標、多離子反應監(jiān)測條件等測定參考參數序號中文名稱保留時間（min）類型定量內標采集模式母離子（m/z）子離子（m/z）碰撞能量（eV）1林可霉素-D33.863內標物1/ESI+410.6129.1*/73.136/762林可霉素3.866目標物1ESI+407.3126.1*/359.340/203呋喃它酮-D54.344內標物2/ESI+330.1286.1*/102.213/134呋喃它酮4.420目標物2ESI+325.1252.0*/281.117/135甲硝唑-D44.691內標物3/ESI+176.282.1*/128.127/146甲硝唑4.749目標物3ESI+172.081.8*/127.725/157金剛烷胺-D155.142內標物4/ESI+167.1150.3*/86.222/258金剛烷胺5.305目標物4ESI+152.1135.1*/107.110/429洛硝達唑5.662目標物5ESI+201.0139.7*/54.610/2510二甲硝咪唑6.596目標物5ESI+142.296.1*/81.918/2011二甲硝咪唑-D36.598內標物5/ESI+145.099.2*/84.018/2412呋喃西林8.515目標物6ESI-197.0149.9*/124.111/1213呋喃西-13C,15N28.517內標物6/ESI-200.2153.1*/82.1/126.29/10/1014甲砜霉素8.788目標物9ESI-354.0185.0*/289.922/1215呋喃妥因9.842目標物7ESI-237.0151.9*/124.117/2016呋喃唑酮-D411.388內標物7/ESI+230.1139.1*/122.116/2217呋喃唑酮11.509目標物7ESI+226.1122.1*/139.121/1518氟甲砜霉素14.822目標物9ESI-356.0336.0*/185.04521919替米考星15.329目標物1ESI+869.5174.1*/696.550/4020紅霉素16.026目標物8ESI+734.3158.1*/576.435/2021紅霉素-13C,D316.027內標物8/ESI+737.4161.2*/579.433/2222氯霉素-D516.083內標物9/ESI-326.0126.0*/157.010/2023泰樂菌素16.102目標物8ESI+916.5174.2*/722.445/3024氯霉素16.106目標物9ESI-321.0152.1*/257.018/1225白霉素16.463目標物8ESI+772.4174.4*/109.135/1526延胡索酸泰妙菌素16.536目標物8ESI+494.3192.1*/119.015/30注：帶*的為定量離子（資料性附錄）方法的精密度和正確度表C.1～C.6中給出了方法的精密度和正確度匯總數據。表C.1精密度匯總表（空白水樣）序號目標化合物加標濃度（ng/L）實驗室內相對標準偏差（%）實驗室間相對標準偏差（%）重復性限（ng/L）再現(xiàn)性限（ng/L）1呋喃唑酮5.009.3~113.9111120.05.1~115.07.67.61006.1~1110.28.88.82呋喃它酮5.006.6~7.9187.47.420.08.2~9.19.38.68.61003.4~6.83.74.86.13呋喃西林5.008.7~1416121220.06.0~9.64.68.28.21003.1~7.87.36.39.74呋喃妥因5.007.5~2013141420.04.5~8.19.37.07.01004.9~7.82.86.26.35紅霉素5.005.3~144.4111120.05.0~112.58.58.51002.7~7.42.65.05.36泰樂菌素5.007.9~150.9121220.04.6~123.88.88.81002.6~8.0126.4137白霉素5.009.1~145.9121220.05.3~121210101006.0~7.94.27.27.98延胡索酸泰妙菌素5.006.2~175.5141420.08.2~11119.59.51005.4~6.34.55.97.29林可霉素5.003.9~138.18.48.420.03.6~113.58.28.21004.2~8.24.66.17.410替米考星5.005.8~173.9131320.06.6~162.811111005.4~6.06.45.78.411氯霉素5.002.8~156.69.69.620.02.3~7.68.75.25.21003.7~9.24.06.47.012甲砜霉素5.004.9~8.96.87.47.420.04.0~148.79.59.51003.5~7.08.95.39.413氟甲砜霉素5.006.1~203.7141420.03.0~11157.27.21006.4~7.34.66.87.414甲硝唑5.004.1~113.27.57.520.05.9~11118.78.71002.9~5.1113.81115二甲硝咪唑5.007.6~135.5111120.08.1~11139.29.21003.2~7.46.26.08.316洛硝達唑5.07.5~1311111120.04.2~9.46.97.17.11003.2~6.77.35.19.517金剛烷胺5.003.9~175.3111120.04.4~9.67.97.57.51003.6~7.06.95.38.8表C.2精密度匯總表（地表水、地下水和海水）序號目標化合物加標濃度（ng/L）實驗室內相對標準偏差（%）實驗室間相對標準偏差（%）重復性限（ng/L）再現(xiàn)性限（ng/L）地表水地下水海水地表水地下水海水地表水地下水海水地表水地下水海水1呋喃唑酮5.006.8~138.0~159.3~142.0128.89.612129.6121220.05.7~128.6~133.3~12137.23.99.4118.69.4118.61004.5~123.2~7.03.7~112.61.21.68.15.27.28.15.27.22呋喃它酮5.002.4~129.9~146.9~154.96.77.67.413117.4131120.08.6~134.8~7.65.7~9.53.79.13.3116.18.2116.18.21003.2~7.52.9~10.61.9~5.96.43.23.45.97.34.58.77.55.43呋喃西林5.008.1~123.1~145.7~8.75.54.16.3119.77.8119.77.820.05.2~123.7~6.25.5~7.37.16.4118.25.36.78.25.36.71004.5~6.34.5~7.93.0~6.45.96.74.95.26.34.77.39.26.74呋喃妥因5.006.2~147.9~146.1~135.1115.711129.711129.720.05.1~142.5~8.53.2~12136.7119.15.47.49.15.47.41003.9~5.91.3~7.45.9~9.28.07.12.84.95.77.39.38.97.35紅霉素5.005.4~167.4~136.5~15123.26.112111112111120.03.7~8.29.7~146.2~8.56.96.44.96.0127.26.0127.21003.9~6.02.8~6.02.9~5.50.70.5114.95.04.14.95.010.46泰樂菌素5.004.3~148.0~155.0~151.67.59.38.712128.7121220.03.3~9.63.6~144.6~13129.37.36.48.99.26.48.99.21005.3~6.92.8~6.55.4~8.33.05.64.96.45.26.56.56.87.67白霉素5.004.3~7.18.9~1414~156.32.0116.312146.3121420.01.9~8.44.5~114.7~5.55.31.06.46.38.55.26.38.55.21003.5~9.13.9~6.84.3~6.36.54.61.76.35.75.48.86.95.48延胡索酸泰妙菌素5.005.7~1111~176.9~155.37.12.88.413118.4131120.07.1~147.0~124.6~8.53.35.97.0118.86.5118.86.51005.6~8.33.4~5.53.6~6.42.09.05.56.74.35.26.710.27.79林可霉素5.007.1~9.88.1~164.1~136.68.85.58.4128.28.4128.220.03.3~6.95.4~9.210~141.54.19.65.98.0125.98.0121003.8~7.03.4~6.82.2~4.55.04.52.25.45.23.46.96.43.710替米考星5.009.6~136.7~136.4~150.22.84.312119.912119.920.05.6~147.4~9.13.8~156.95.15.5118.49.8118.49.81005.1~5.65.0~6.12.7~9.55.48.36.85.45.66.77.49.48.711氯霉素5.0011~122.7~115.2~154.93.85.1128.29.9128.29.920.07.0~149.7~124.8~8.27.65.17.211116.611116.61002.1~5.93.9~7.02.8~4.61.34.45.74.25.53.74.26.86.512甲砜霉素5.006.9~139.1~155.4~9.96.83.28.69.9137.99.9137.920.07.5~125.9~7.45.3~9.83.71.64.89.57.07.59.57.07.51002.5~7.34.8~112.5~6.71.6123.84.97.54.54.9135.913氟甲砜霉素5.005.7~9.85.1~156.4~186.15.83.88.311128.3111220.06.0~105.7~9.14.7~9.45.88.57.48.08.07.08.08.07.01002.8~6.34.0~9.72.3~7.73.8116.84.87.05.35.8128.814甲硝唑5.006.6~146.1~167.8~129.47.95.611129.711129.720.04.4~8.74.4~134.7~114.76.45.37.38.68.37.38.68.31002.7~7.23.4~6.03.8~6.99.73.45.65.25.05.5125.87.515二甲硝咪唑5.009.4~136.7~139.1~135.38.83.811111111111120.06.3~115.8~119.6~144.64.9138.79.1138.79.1131004.7~8.74.2~7.45.8~8.01.94.73.57.05.66.87.06.97.016洛硝達唑5.007.4~145.5~156.0~114.75.72.5129.58.8129.58.820.04.9~6.26.1~117.6~9.35.74.65.85.78.08.85.78.08.81006.0~9.91.9~6.74.4~7.23.2102.97.85.66.27.8126.317金剛烷胺5.008.0~1412~197.2~165.76.90.111151411151420.05.1~195.1~1511~136.8152.6129.412129.4121004.3~7.22.8~5.96.7~8.08.93.84.25.94.87.6116.18.2表C.3精密度匯總表（廢水）序號目標化合物加標濃度（ng/L）實驗室內相對標準偏差（%）實驗室間相對標準偏差（%）重復性限（ng/L）再現(xiàn)性限（ng/L）1呋喃唑酮20.06.8~9.39.47.97.940.011~141112121601.2~6.85.74.9112呋喃它酮20.08.5~143.3111140.06.5~8.15.67.27.21603.7~6.4125.3203呋喃西林20.03.6~7.91.05.85.840.03.2~6.84.45.05.01602.0~4.54.43.87.54呋喃妥因20.07.2~1612121240.04.3~111.17.87.81600.7~7.07.25.6125紅霉素20.06.4~12128.98.940.05.8~9.66.58.08.01603.0~3.98.83.4146泰樂菌素20.012~1510141440.03.3~11136.97.71601.5~9.26.05.9117白霉素20.013~164.3141440.08.1~9.6138.99.21601.5~6.7114.8198延胡索酸泰妙菌素20.08.1~117.49.59.540.06.9~174.912121602.3~6.0115.0209林可霉素20.09.7~142.7121240.07.6~135.811111602.8~8.2126.71810替米考星20.05.6~6.03.15.95.940.05.6~6.6156.28.01604.3~7.5176.52511氯霉素20.05.6~144.69.49.440.03.3~8.01.56.16.11600.9~6.22.94.26.112甲砜霉素20.06.8~124.4111140.03.7~9.12.67.17.11602.8~5.15.53.89.613氟甲砜霉素20.07.7~156.5121240.06.6~8.93.57.97.91602.6~140.68.98.914甲硝唑20.06.5~123.59.09.040.04.5~115.37.37.31602.5~6.72.35.15.915二甲硝咪唑20.08.6~135.8111140.05.9~9.82.67.47.41601.1~6.11.94.35.016洛硝達唑20.011~1313121240.05.0~9.66.68.28.21602.0~4.6133.31917金剛烷胺20.012~205.5161640.06.7~105.38.08.01602.3~8.5115.419表C.4正確度匯總表（空白水樣）序號目標化合物加標濃度（ng/L）回收率范圍（%）P±21呋喃唑酮5.0091.8~99.495.8±7.620.090.6~99.596.2±9.810086.8~10598.6±20.42呋喃它酮5.0080.8~113101±34.620.094.6~114106±20.0100110~118115±8.03呋喃西林5.0085.8~118104±32.520.0108~114112±6.9100101~117108±15.34呋喃妥因5.0087.7~112103±25.920.086.8~10497.4±18.510094.6~99.897.0±5.35紅霉素5.0089.6~97.694.2±8.220.093.0~97.594.7±4.910099.4~104101±5.36泰樂菌素5.0097.0~98.898.0±1.820.089.8~96.392.3±7.010085.6~10693.3±22.17白霉素5.00103~115108±12.320.094.6~112105±17.7100103~111108±8.28延胡索酸泰妙菌素5.0091.6~10194.7±10.320.091.4~10598.4±13.610099.9~109105±9.39林可霉素5.0093.6~111102±16.520.0103~110107±6.7100102~111106±10.210替米考星5.00109~117113±8.820.099.7~106103±6.410096.2~110103±13.911氯霉素5.0092.6~106101±13.820.095.6~114104±17.810092.4~99.696.7±7.612甲砜霉素5.0089.6~10294.7±13.020.087.1~10495.4±16.910084.0~10091.2±16.313氟甲砜霉素5.0087.3~93.990.9±6.720.080.6~10488.8±26.310083.7~91.687.4±8.014甲硝唑5.0097.3~104101±6.320.097.0~108103±11.010085.9~10697.1±20.315二甲硝咪唑5.0092.0~10397.8±10.820.086.0~11097.2±24.110098.4~110103±13.416洛硝達唑5.089.3~111102±21.620.0104~113108±9.2100106~119113±13.117金剛烷胺5.00106~116110±10.820.0103~110106±7.210099.7~112106±12.3表C.5正確度匯總表（地表水、地下水和海水）序號目標化合物加標濃度（ng/L）地表水地下水海水回收率范圍（%）P±2回收率范圍（%）P±2回收率范圍（%）P±21呋喃唑酮5.00101~105103±4.286.0~10798.7±22.499.0~116105±19.220.083.9~10995.5±24.694.8~109101±14.495.3~10398.6±7.910097.4~103101±6.095.6~97.996.9±2.498.1~10299.9±3.92呋喃它酮5.0095.7~10599.3±10.093.3~10698.6±13.291.4~105101±15.720.097.8~106103±7.799.1~118108±19.6101~108104±7.2100102~115108±13.0103~110107±6.497.8~105103±7.83呋喃西林5.0092.2~10396.4±11.696.7~105102±8.295.6~108102±12.620.092.0~10799.7±14.294.2~107102±13.093.2~114106±21.210090.7~10295.5±11.7102~115107±13.4101~111105±9.74呋喃妥因5.0089.9~99.095.4±9.796.3~119109±22.893.3~10598.2±12.120.093.7~117103±24.799.6~114108±14.490.8~112101±21.410093.5~110103±16.493.9~109101±15.289.9~95.092.7±5.15紅霉素5.0086.1~10895.7±22.499.6~107103±6.597.3~110105±13.020.090.6~10496.3±13.8106~119111±13.594.4~10498.5±9.810094.9~96.195.4±1.394.5~95.494.9±0.981.5~10191.6±19.56泰樂菌素5.0090.7~93.592.3±2.993.3~107103±15.589.3~10899.0±18.820.078.5~97.686.3±20.194.7~115106±19.882.8~95.690.1±13.210092.3~97.995.3±5.682.6~91.988.2±9.990.4~99.295.8±9.57白霉素5.0085.1~96.091.7±11.699.3~103102±4.388.4~10795.1±20.620.0107~117111±10.6104~106106±2.381.5~91.688.1±11.310093.9~106102±13.495.9~105101±9.099.3~103102±3.58延胡索酸泰妙菌素5.0082.5~90.687.8±9.3101~115110±14.7110~116114±5.620.0103~109105±6.4102~114108±11.690.6~10395.0±13.910098.3~103101±4.095.2~114105±18.8103~115110±11.79林可霉素5.0081.5~91.988.2±11.692.3~109100±16.992.3~109100±16.920.099.2~102102±3.388.5~10899.2±19.788.5~10899.2±19.710090.5~10195.4±10.691.7~95.793.8±4.091.7~95.793.8±4.010替米考星5.0099.4~99.999.6±0.5102~108106±7.091.4~99.695.4±8.220.089.7~10397.1±13.593.1~10498.6±10.985.0~94.490.7±10.010096.8~108104±11.290.7~10595.7±15.985.4~97.590.8±12.311氯霉素5.0090.1~99.395.1±9.398.5~109103±10.990.9~10196.1±10.120.088.8~10297.6±15.294.6~10799.2±12.986.3~99.793.2±13.4100103~106105±2.696.4~105102±9.094.6~10699.0±12.212甲砜霉素5.0092.0~10699.1±14.0106~112109±6.497.2~115108±18.820.095.0~10398.9±8.096.1~99.097.9±3.1105~115109±10.610099.6~103101±3.783.3~10493.3±20.7106~114111±8.413氟甲砜霉素5.0095.4~108103±12.4102~118110±15.092.3~109100±16.920.099.0~110103±12.593.0~114102±21.588.5~10899.2±19.710094.3~10298.5±7.884.1~10395.3±19.991.7~95.793.8±4.014甲硝唑5.0093.7~110105±18.896.6~113105±16.393.5~104101±11.820.099.7~105103±5.796.6~110104±13.495.5~106103±11.610097.2~111103±15.098.9~106102±8.096.1~108102±12.115二甲硝咪唑5.0092.5~10295.9±10.795.3~114105±18.492.3~109100±16.920.0102~111106±10.595.1~10599.9±9.988.5~10899.2±19.710094.5~98.095.8±3.894.3~10499.8±9.991.7~95.793.8±4.016洛硝達唑5.0093.8~10498.9±9.4104~117110±12.395.7~10198.4±5.320.093.1~104101±12.0103~112107±9.496.4~108102±11.710090.8~96.893.7±6.093.8~115106±21.099.1~105103±6.017金剛烷胺5.00108~113111±4.8102~108106±6.0103~109106±6.020.088.0~10294.1±14.483.3~95.289.6±11.9108~114111±