分級凈化結(jié)合氣相色譜質(zhì)譜聯(lián)用法測定豆芽中10種植物生長調(diào)節(jié)劑

吳平谷等

摘 要 建立了豆芽10種植物生長調(diào)節(jié)劑的分級凈化體系，

1 引 言

我國豆芽以作坊式生產(chǎn)為主，在豆芽生產(chǎn)過程中肆意添加植物生長調(diào)節(jié)劑催發(fā)豆芽生長常有發(fā)生，添加的植物生長調(diào)節(jié)劑主要有等。本研究針對豆芽生產(chǎn)過程中可能使用的10種植物生長調(diào)節(jié)劑，通過加標實驗，根據(jù)其化學性質(zhì)進行分級凈化，采用氣相色譜質(zhì)譜法對該凈化體系的進行了評價，獲得較好的凈化效果，有較大實際應用價值。

2 實驗部分

2.1 儀器與試劑

3.5 樣品分析

從杭州超市、農(nóng)貿(mào)市場中采集豆芽各10份進行10種植物生長調(diào)節(jié)劑殘留分析，主要檢出CPA和吲哚乙酸，檢出率

分別為50%和20%，含量范圍為0.014～0.26 mg/kg，，CPA已經(jīng)從GB27622011《食品安全國家標準 食品添加劑使用標準》中刪除了在豆芽生產(chǎn)中使用的規(guī)定。吲哚乙酸是植物內(nèi)源性生長素之一，可以促進豆芽桿的生長，未見豆芽中吲哚乙酸本底含量的報道，雖然吲哚乙酸對動物的毒性較低， 目前我國尚未規(guī)定吲哚乙酸在豆芽生產(chǎn)中應用。

References

1 SU FangFei， HU MengQing， MEI TianZi， YANG Bei， YANG ShuLong ， ZOU WeiYing， ZOU Ting， ZHANG DaLei. Journal of Nanchang University（Medical Science）， 2013， 53（1）： 13-15

蘇芳菲 ， 胡夢青 ， 梅天資， 楊 蓓 ， 楊樹龍 ， 鄒惟瑩 ， 鄒 挺 ， 張大雷. 南昌大學學報（醫(yī)學版）， 2013， 53（1）： 13-15

2 XU AiDong. China Vegetables， 2009 （8）： 1-6

徐愛東. 中國蔬菜， 2009 （8）： 1-6

3 WANG YiQian， ZHANG GuangHua， HE HongJu. Modern Instruments， 2012， 18（2 ）： 6-10

王一茜， 張廣華， 何洪巨， 現(xiàn)代儀器， 2012， 18（2 ）： 6-10

4 GB/T232052008 Determination of 448 pesticides and related chemicals residues in tea LCMSMS method. National Standards of the People′s Republic of China

茶葉中448種農(nóng)藥多殘留及相關(guān)化學品殘留量的測定 液相色譜質(zhì)譜法， 中華人民共和國國家標準 GB/T232052008

5 LIU JingJing， GONG Ping， ZHANG XiaoMei， WANG JianHua， WANG JingTang. Chinese Journal of Chromatography， 2012， 30（10）： 1012-1016

劉靖靖， 宮 萍， 張曉梅， 王建華， 王境堂. 色譜， 2012， 30（10）： 1012-1016

6 MOU YanLi，GUO DeHua，DING ZhuoPing，YI XiongHai. Chinese J. Anal. Chem.， 2013， 41（11）： 1640-1646

牟艷莉， 郭德華， 丁卓平， 伊雄海. 分析化學， 2013， 41（11）： 1640-1646

7 WU FengQi， JIN BaoHui， CHEN Bo， CHEN PeiJin， XIAO Feng. Chinese Agricultural Science Bulletin， 2010， 26（15）： 115119

吳鳳琪， 靳保輝， 陳 波， 陳沛金， 肖 鋒. 中國農(nóng)學通報， 2010， 26（15）： 115-119

8 MOU YanLi， GUO DeHua， DING ZhuoPing， Journal of Instrumental Analysis， 2013， 32（8）： 935-940

牟艷利， 郭德華， 丁卓平. 分析測試學報， 2013， 32（8）： 935-940

9 Ma L， Zhang H， Xu W， He X， Yang L， Luo Y， Huang K. Food Anal. Methods， 2013， 6（3）： 941-951

10 Zhang F， Zhao P， Shan W， Gong Y， Jian Q， Pan C. Bull Environ Contam Toxicol， 2012， 89： 674-679

11 Anastasslades M， Lehotay S J， Stajnbaher D. J. AOAC International， 2003， 86（2）： 412-431

12 ZHAO YanSheng， DONG Ying， ZHANG Feng， YANG MinLi， FENG Feng， CHU XiaoGang Chinese J. Anal. Chem.， 2012， 40（2）： 249-256

趙延勝， 董 英， 張 峰， 楊敏莉， 馮 峰， 儲曉剛. 分析化學， 2012， 40（2）： 249-256

13 WU PingGu， WANG Qiang， CHEN HuiHua， YING YongFei， ZHAO YongXin . Chinese J. Anal. Chem.， 2008， 36（11）： 1476-1482

吳平谷， 王 強， 沈向紅， 陳慧華， 宋國良， 應永飛， 徐小民， 趙永信.分析化學， 2008， 36（11）： 1476-1482

Determination of 10 Plant Growth Regulators in Bean Sprouts by

Sequential CleaningGas ChromatographyMass Spectrometry

WU PingGu， TAN Yin， ZHANG Jin， WANG LiYuan， TANG Jun，

JIANG Wei， PAN XiaoDong， MA BingJie， NI ZhuNan， WANG TianJiao

（Zhejiang Provincial Center for Disease Control and Prevention， Hangzhou 310051， China）

Abstract A sequential cleanup method was developed for the quantification of 10 plant growth regulators in bean sprout by the gas chromatography/mass spectrometry （GC/MS）. The analytes were firstly extracted by the acided acetonitrile. Extraction was concentrated and redissovled by methanol. Then， it was divided to two aliquots. One of that was analyzed for 2，4Dbutyl ester and 2，4Dethyl ester after the purification by QuECHERS cartridge. Another one was treated by MCS solid phase extraction column including diverse eluting steps. After eluting by 5 mL methanol， composition 1 was obtain， concentrated， and methyl esterified by 10% boron trifluoride methanol solution. The treated extract was used for the determination of 4chlorophenoxy acetic acid， βnaphthyl acetic acid， 2，4dichlorophenoxy acetic acid， indole acetic acid and indole butyric acid. Composition 2 collected by eluting with 5 mL 5% amonium methanol was used for the determination of paclobutrazol， Kinetin， 6Benzylaminopurine. The cleanup procedures are designed according to different chemistry properties of these plant growth regulators. The results showed that after spiking of 0.01-0.1 mg/kg selected plant growth regulators， average recovery ranged from 70.0% to 93.2% and relative standard deviation were 5.2%-12.3%. Limit of quantification （LOQ S/N≥10） and limit of detection （LOD S/N≥3） were 0.01-0.025 mg/kg and 0.003-0.008 mg/kg respectively. The developed purification method is easy， fast and accurate， and can be applied to routine test of plant growth regulators in bean sprout.

Keywords Bean sprout； Plant growth regulator； Sequential cleaning； Gas chromatographymass spectrometry

（Received 3 February 2014； accepted 17 March 2014）

吳平谷， 王 強， 沈向紅， 陳慧華， 宋國良， 應永飛， 徐小民， 趙永信.分析化學， 2008， 36（11）： 1476-1482

Determination of 10 Plant Growth Regulators in Bean Sprouts by

Sequential CleaningGas ChromatographyMass Spectrometry

WU PingGu， TAN Yin， ZHANG Jin， WANG LiYuan， TANG Jun，

JIANG Wei， PAN XiaoDong， MA BingJie， NI ZhuNan， WANG TianJiao

（Zhejiang Provincial Center for Disease Control and Prevention， Hangzhou 310051， China）

Abstract A sequential cleanup method was developed for the quantification of 10 plant growth regulators in bean sprout by the gas chromatography/mass spectrometry （GC/MS）. The analytes were firstly extracted by the acided acetonitrile. Extraction was concentrated and redissovled by methanol. Then， it was divided to two aliquots. One of that was analyzed for 2，4Dbutyl ester and 2，4Dethyl ester after the purification by QuECHERS cartridge. Another one was treated by MCS solid phase extraction column including diverse eluting steps. After eluting by 5 mL methanol， composition 1 was obtain， concentrated， and methyl esterified by 10% boron trifluoride methanol solution. The treated extract was used for the determination of 4chlorophenoxy acetic acid， βnaphthyl acetic acid， 2，4dichlorophenoxy acetic acid， indole acetic acid and indole butyric acid. Composition 2 collected by eluting with 5 mL 5% amonium methanol was used for the determination of paclobutrazol， Kinetin， 6Benzylaminopurine. The cleanup procedures are designed according to different chemistry properties of these plant growth regulators. The results showed that after spiking of 0.01-0.1 mg/kg selected plant growth regulators， average recovery ranged from 70.0% to 93.2% and relative standard deviation were 5.2%-12.3%. Limit of quantification （LOQ S/N≥10） and limit of detection （LOD S/N≥3） were 0.01-0.025 mg/kg and 0.003-0.008 mg/kg respectively. The developed purification method is easy， fast and accurate， and can be applied to routine test of plant growth regulators in bean sprout.

Keywords Bean sprout； Plant growth regulator； Sequential cleaning； Gas chromatographymass spectrometry

（Received 3 February 2014； accepted 17 March 2014）

吳平谷， 王 強， 沈向紅， 陳慧華， 宋國良， 應永飛， 徐小民， 趙永信.分析化學， 2008， 36（11）： 1476-1482

Determination of 10 Plant Growth Regulators in Bean Sprouts by

Sequential CleaningGas ChromatographyMass Spectrometry

WU PingGu， TAN Yin， ZHANG Jin， WANG LiYuan， TANG Jun，

JIANG Wei， PAN XiaoDong， MA BingJie， NI ZhuNan， WANG TianJiao

（Zhejiang Provincial Center for Disease Control and Prevention， Hangzhou 310051， China）

Abstract A sequential cleanup method was developed for the quantification of 10 plant growth regulators in bean sprout by the gas chromatography/mass spectrometry （GC/MS）. The analytes were firstly extracted by the acided acetonitrile. Extraction was concentrated and redissovled by methanol. Then， it was divided to two aliquots. One of that was analyzed for 2，4Dbutyl ester and 2，4Dethyl ester after the purification by QuECHERS cartridge. Another one was treated by MCS solid phase extraction column including diverse eluting steps. After eluting by 5 mL methanol， composition 1 was obtain， concentrated， and methyl esterified by 10% boron trifluoride methanol solution. The treated extract was used for the determination of 4chlorophenoxy acetic acid， βnaphthyl acetic acid， 2，4dichlorophenoxy acetic acid， indole acetic acid and indole butyric acid. Composition 2 collected by eluting with 5 mL 5% amonium methanol was used for the determination of paclobutrazol， Kinetin， 6Benzylaminopurine. The cleanup procedures are designed according to different chemistry properties of these plant growth regulators. The results showed that after spiking of 0.01-0.1 mg/kg selected plant growth regulators， average recovery ranged from 70.0% to 93.2% and relative standard deviation were 5.2%-12.3%. Limit of quantification （LOQ S/N≥10） and limit of detection （LOD S/N≥3） were 0.01-0.025 mg/kg and 0.003-0.008 mg/kg respectively. The developed purification method is easy， fast and accurate， and can be applied to routine test of plant growth regulators in bean sprout.

Keywords Bean sprout； Plant growth regulator； Sequential cleaning； Gas chromatographymass spectrometry

（Received 3 February 2014； accepted 17 March 2014）